ZLD solution for Pharmaceutical Industry

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ZLD solution for Pharmaceutical Industry Hemant Wagh Associate Vice President Water & WW solutions Group

Major Concerns... Where is the space for process plant??? Can I generate/save energy??? Can I use treated wastewater somewhere??? Can I avoid liquid discharge??? Reduce Foot Print, Recycle Wastewater, ZLD, Energy Recovery

Solutions... Selection of Appropriate Technologies Integrated Design Approach Solution under one roof for ZLD

Challenges Accurate data TDS Determines Evaporation Duty Determines Salt Handling Capacity Organic Matter Determines Purity Of Salt Determines Process Condensate COD & BOD Determines Organic Cut from Evaporation Compositional Analysis Characteristic @various Concentration Pure Salt Vs. Mixed Salt Recovery Process Schematics Operating Parameters MOC compatibility Selection Of Type of Evaporators Selection of Process Schematics www.praj.net Confidential 4

Design Considerations Temperature scaling flow ability issues due to viscosity and salt solubility Corrosion Effluent Composition Selection of Type of Evaporators Energy Consumption Organic Cut Auxiliary Evaporators Load Mixed Salt quantity Boiling Point Elevation in Evaporators Crystallization Methodology Utility Requirements Operating Cost Choking Issues and Salt Dryness www.praj.net Confidential 5

Typical comparison Offerings Features/Applications Advantage Benefits & Limitations Falling Film Evaporators Effluents with Low TSS, Low hardness & Silica Higher Heat Transfer Coefficient Less Power Consumption, Not suitable for highly viscous liquids Forced Film Evaporators Effluents with High TSS, high hardness & silica Reduction in CIP Frequency, Suitable for High Viscous Effluents Low Scaling Tendency due high Tube Velocity, High operating cost TVR Acts as additional effect Increase in Steam Economy Reduces Operating Cost. Cant recover pure steam condensate MVR Where steam is not available/steam generation cost is high, Operates on Power No steam is required during operation Beneficial where power is surplus. Higher Capex Pusher Centrifuge Concentrate from MEE is treated in PC. End product is salt Crystalline salts can be separated easily Simple in Operation, Lower Capex & Opex. Amorphous salt cant be separated ATFD - EcoDry To convert concentrate from MEE to dry powder. Zero Clearance Hinged Scrapping Blades No chemical CIP required, Higher Heat Transfer Coefficient Moisture content <8 to 10% Very less mechanical break down As end unit operation opex is high 6

Solvent Recovery - Stripping Praj Patented Rh Grid trays are compatible to TSS load up to 2000 ppm without affecting performance Most effective on multiple feed inlet, gives flexibility in operation depending on variation in feed condition In Tray column the pressure drop is comparatively less hence less steam consumption Software design like CHEMCAD helps in getting accurate Process results

Chemcad Simulation NH 3 & SOLVENT Stripper Praj Industries Ltd www.praj.net 8

General API Effluent Pharma API effluent ML Stream ( High COD High TDS Stream) FROM PLANT Product Separation First washing of reactors Traces of solvents & Ammonia from Plant Lean Stream ( Low COD Stream) FROM PLANT Reactor Washings (2 nd washing onwards) UTILITY WASTE DM Plant Regeneration RO water Reject Cooling Tower blow down Boiler blow down OTHER Floor washing Praj Industries Ltd www.praj.net 9

Typical Recycle & ZLD scheme Cooling towers Blow Down effluent/reactor washings MGF Clarification systems Solvent Stream Cooling Tower Make up water Low TSS / TDS and Low Hardness water UF - RO Based systems Solvent recovery Salt for disposal ATFD Multiple Effect Evaporator Reject RO 10

EXPECTED SOLVENTS IN EFFLUENT FROM PHARMA API EFFLUENT Solvent Boiling Point (ºC) Acetic Acid 118.0 Acetic Acid Anhydride 139.0 Acetone 56.3 Acetonitrile 81.6 Benzene 80.1 iso-butanol 107.7 n-butanol 117.7 tert-butanol 82.5 Carbon Tetrachloride 76.5 Chlorobenzene 131.7 Chloroform 61.2 Cyclohexane 80.7 Cyclopentane 49.3 Dichloromethane 39.8 Diethyl Ether 34.6 Dimethyl Acetamide 166.1 Dimethyl Formamide 153.0 Dimethyl Sulfoxide 189.0 Dioxane 101.0 Praj Industries Ltd www.praj.net Solvent Boiling Point (ºC) Ethyl Ether 34.6 Ethylene Dichloride 83.5 Ethylene Glycol 197.5 Heptane 98.4 n-hexane 68.7 Hydrochloric Acid 84.8 Methanol 64.7 Methylene Chloride 39.8 MTBE 55.2 Pentane 36.1 Petroleum Ether 35.0-60.0 iso-propanol 82.3 n-propanol 97.2 Pyridine 115.3 Tetrahydrofuran 66.0 Toluene 110.6 Trifluoroacetic Acid 71.8 Water 100.0 Xylene 140.0 11

Typical API Parameters High COD High TDS Stream Parameters Unit Concentration ph 1-14 TDS ppm 5000-6000 COD ppm 60000 150000 Ammoniacal Nitrogen ppm 500-900 Solvents (Methanol. IPA, Toluene, MDC, TBME, Ethyl Acetate, DMSO, DMF, Heptane, Hexane, THF) % 5-12% Lean Stream ( Low COD Stream) Parameters Unit Concentration ph 7-8 TDS ppm 3000-4000 COD ppm 3500 5000 BOD ppm 1500 2000 Ammoniacal Nitrogen ppm 50-100 Praj Industries Ltd www.praj.net 12

Typical Issues - Pharma API Effluent 1. Large Variations in Parameters & Shock Loads Results in under performance of plant & inefficient operations. 2. Variations in Solvent Mix based on the Product mix Inefficient operation of Stripper affecting MEE & contaminated Process Condensate 3. TDS composition Varies & is difficult to predict Inconsistent operations of MEE 4. Wide variation in Hardness & Silica levels - Frequent Scaling & down time for cleaning 5. Ammoniacal Nitrogen - Affects the down stream MEE & Process Condensate quality 6. Design of UF/RO Recycle Plant Inconsistent Operations & frequent fouling Praj Industries Ltd www.praj.net 13

Pharma Case Study Praj Industries Ltd www.praj.net

Thermo Multiple Vapor Effect Recompression Evaporation Motive Steam STEAM FEED 2 EFFECTS WITH FALLING FILM AND 3 rd EFFECT WITH FORCED CIRCULATION

Design Features If both streams are mixed, steam condensate of the MEE can not be reused due to TVR. The condensate might have contaminated with solvents Due to above reason, it was decided to go for separate MEEs for RO Reject & ML Also, as Ammonical Nitrogen effluent may not be component of all streams, it was decided to strip it separately using Ammonia Stripper at high ph

Final Scheme RO PERMEATE EXISTING ETP RO RO Reject MEE MEE CONDENSATE RO REJECT 2% solids RO MEE STREAM 40% TDS ML STREAM 13% TDS SOLVENT STRIPPER Ammonia STRIPPER STRIPPER BOTTOM ML MEE ML MEE STREAM 40% TDS ATFD DRY SOLIDS

Plant photographs Torrent Pharmaceuticals Ltd, India Calandria Stripper Column MEE Plant Praj Industries Ltd www.praj.net 18

Plant photographs ZLD Plant Agitated Thin Film Dryer (ATFD) Praj Industries Ltd www.praj.net 19

Plant photographs ATFD Dry Powder Video Dry Powder 20

Praj An Overview LEED Platinum Certified Green Building 21

Praj - Overview Experience Solutions Presence Certification Standards > 30 years in Distillery, Power, Pharma, Chemicals, Ferrous & Non ferrous, Food & Beverages, Textiles. WTP, ETP, Effluent Recycling systems (ERS) & Zero Liquid Discharge (ZLD) Over 65 countries across the globe, Listed on BSE & NSE ISO 9001:2008 (Certification by Bureau Veritas), U Stamp, U2, ISO 14001:2008 ASME Sec VIII Div. I, IS 2825, TEMA, DIN, API 650 Developing sustainable solutions to transform the world s most difficult waters into valuable resources 22

Pune Kandla Wada Manufacturing Capability Domestic Unit Fabrication capacity - 6000 MT/Year SEZ Units 1&2 SEZ Unit 2 - high thickness vessels Fabrication capacity - 5000 MT/Year US FDA, UK MHRA and WHO compliant systems 23

Key References And Many More Praj Industries Ltd www.praj.net 24

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