ZLD solution for

Pharmaceutical Industry

Hemant Wagh Associate Vice President

Water & WW solutions Group

Where is the

space for

process

plant???

Reduce Foot Print, Recycle Wastewater, ZLD, Energy

Recovery

Major Concerns. . .

Can I use treated

wastewater

somewhere???

Can I avoid liquid

discharge???

Can I

generate/save

energy???

Integrated Design Approach

Selection of Appropriate Technologies

Solution under one roof for ZLD

Solutions. . .

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• Determines Evaporation Duty

• Determines Salt Handling Capacity TDS

• Determines Purity Of Salt

• Determines Process Condensate COD & BOD

• Determines Organic Cut from Evaporation

Organic Matter

• Pure Salt Vs. Mixed Salt Recovery

• Process Schematics

• Operating Parameters

• MOC compatibility

Compositional Analysis

• Selection Of Type of Evaporators

• Selection of Process Schematics

Characteristic @various

Concentration

4

Challenges – Accurate data

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• scaling

• flow ability issues due to viscosity and salt solubility

• Corrosion

Temperature

• Selection of Type of Evaporators

• Energy Consumption

Effluent Composition

• Auxiliary Evaporators Load

• Mixed Salt quantity

• Boiling Point Elevation in Evaporators Organic Cut

• Utility Requirements

• Operating Cost

• Choking Issues and Salt Dryness

Crystallization

Methodology

5

Design Considerations

Typical comparison

6

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

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

Solvent Recovery - Stripping

Chemcad Simulation

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NH3 & SOLVENT Stripper

General API Effluent

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Pharma API effluent

Lean Stream ( Low COD

Stream)

ML Stream ( High COD – High

TDS Stream)

FROM PLANT

Reactor Washings (2nd washing

onwards)

UTILITY WASTE

DM Plant Regeneration

RO water Reject

Cooling Tower blow down

Boiler blow down

FROM PLANT

Product Separation

First washing of reactors

Traces of solvents & Ammonia

from Plant

OTHER

Floor washing

10

Cooling

towers

Blow Down

effluent/reactor

washings

Low TSS / TDS

and Low

Hardness water

MGF

Clarification

systems

UF - RO Based

systems

Cooling Tower

Make up water

Multiple

Effect

Evaporator

Reject RO Salt for

disposal ATFD

Typical Recycle & ZLD scheme

Solvent

Stream

Solvent

recovery

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www.praj.net 11

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

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

EXPECTED SOLVENTS IN EFFLUENT FROM PHARMA API EFFLUENT

Typical API Parameters

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Parameters Unit Concentration

pH 7-8

TDS ppm 3000 - 4000

COD ppm 3500 – 5000

BOD ppm 1500 – 2000

Ammoniacal

Nitrogen

ppm 50-100

Lean Stream ( Low COD 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%

High COD – High TDS Stream

Typical Issues - Pharma API Effluent

© Praj Industries Ltd www.praj.net 13

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

Pharma Case Study

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Thermo Vapor Recompression

FEED

STEAM

2 EFFECTS WITH FALLING FILM AND 3rd EFFECT WITH FORCED CIRCULATION

Multiple Effect Evaporation Motive Steam

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

EXISTING ETP

RO

RO Reject MEE

RO PERMEATE

DRY SOLIDS

ML STREAM 13% TDS

SOLVENT STRIPPER

ML MEE

MEE CONDENSATE

STRIPPER BOTTOM

ATFD

RO REJECT 2% solids

ML MEE STREAM 40% TDS

Ammonia STRIPPER

RO MEE STREAM 40% TDS

Torrent Pharmaceuticals Ltd, India

© Praj Industries Ltd www.praj.net 18 MEE Plant

Calandria

Stripper Column

Plant photographs

Plant photographs

© Praj Industries Ltd www.praj.net 19

ZLD Plant Agitated Thin Film Dryer (ATFD)

20

Plant photographs

Dry Powder

ATFD Dry Powder Video

21

Praj – An Overview

LEED Platinum Certified Green Building

22

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

Praj - Overview

23

Manufacturing Capability Pune

Domestic Unit

Fabrication capacity - 6000 MT/Year

Kandla

SEZ Units 1&2

SEZ Unit 2 - high thickness vessels

Fabrication capacity - 5000 MT/Year

Wada

US FDA,

UK MHRA and WHO compliant systems

Key References

24 © Praj Industries Ltd www.praj.net

And Many More……

Think Forward!