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Continuous Flow ReactorsFixed-bed Tubular Reactors

™Flow Chemistry Specialist

®

• Inconsistent batch performance due to high sensitivity towards process variables (temperature, pressure, concentration, time and mixing)

• Process needs- High heat transfer area- Efficient mixing- Rapid mass transfer- High interfacial area

• Safety issues in- Storing large inventories of hazardous reactants- Handling of hazardous and unstable chemicals- Generation of unstable intermediate by-products during the reaction- Containing unwanted runaway

• Process waste related issues- Need for enhancing the selectivity close to theoretical value- Generation of waste that needs treatment- Need to avoid or reduce the downstream processing efforts for purification

• Distributed production- Produce only as per the local requirement/ consumption (Location wise production)- Produce only as and when needed (avoid inventories)

• Optimal utilization of facility- A continuous flow manufacturing facility can also be used for production of multiple products with almost same

peripherals- Space occupancy will be less- Achieve same or even better than conventional batch operation

Guidelines on when to use AMaR series of flow reactors

About AMAR Serving Industry Since 1974

ISO, CE, PED, ASME, UL, CSA, ex-proof certification

Largest mfgr. & exporter of flow reactors in India

Exports to over 50 countries worldwide

40 distributors worldwide for local support

Largest mfgr. & exporter of autoclave / reactors in India

Manufacturing on CNC/VMC & automated machines

Quality & certified components used

Metal microreactors in technical collaboration with NCL Pg. 1-5

Glass microreactors of LTF-Germany Pg. 6-7

Fixed bed tubular reactors Pg. 8-11

Malshe's interchangeable vapor phase reactor Pg. 11

Optional accessories Pg. 12-13

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Transform your process development capabilities using AMaR series continuous flow reactors

AMaR series is ideal for carrying out a wide range of chemical reactions in the field of pharmaceuticals, fine and specialty Chemicals in a continuous manner.

Applications

Suitable for• Homogeneous reactions: Neutralization, condensation, dehydration reactions etc.• Multiphase Reactions:

- Gas-liquid reactions (G-L): oxidation, ozonolysis, halogenation, chlorination, etc. - Liquid-liquid reactions (L-L): nitration, diazotization, azo coupling, transfer hydrogenation, sulfoxidation, amination, nitration of aromatic substrate, acylation, formylation, methylation, synthesis of nanomaterials, knoevenagel condensation, meerwein arylation, glycosylation reaction, hydrolysis, alkylation etc. - G-L-S and L-S catalytic reactions: esterification, hydrogenation, condensation etc.

• Extraction and separation of Co from Ni using AMaR-3

The devices developed under AMaR series are designed to offer excellent mixing and heat transfer for carrying out fast and exothermic reactions. The design is based on extensive experiments as well as years of research on flow and transport processes carried out at CSIR-National Chemical Laboratory, Pune. The geometry is selected in a manner that while they offer high heat transfer area per unit reactor volume, they also allow flow of dilute suspension of nano-catalysts. The channels / tubes may also be packed with catalyst for catalytic reactions.

Key design attributes

• Better mixing & very high heat transfer area per unit volume.

• Faster reactions & better selectivity.

• Higher yield.

• High safety & ideal for exothermic reactions.

• Reduced waste and faster transfer of process from laboratory to pilot/commercial scale manufacturing.

• Easily scaleable

Advantages of continuous flow reactors over batch reactors:

•

• Microchannels with modular system to connect multiple reactors in series or parallel

• Pressures up to 350 bar & temperatures up to 500°C

• Flow rates up to 500 LPH per unit

• MOC: SS316, Hastelloy, Inconel, Monel, Titanium, Tantalum lined etc.

• Suitable for various liquid-liquid, gas-liquid homogeneous - multiphase reactions, gas, solid & liquid catalytic reactions

Available in integrated multilayer & tubular metal construction for reaction & heat transfermixing,

A M a R mar icro-mixer nd eactor (In technical collaboration with CSIR-NCL)

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• Continuous flow meerwein arylation J. Flow Chem. 2014, 4(4), 211-216

• Continuous flow synthesis of regioregular poly (3-hexythiophene)Ultrafast polymerization with high throughput and low polydispersity indexJ. Flow Chem. 2014, 4(4), 206-210

• 3D Flow Reactors: Flow, Hydrodynamics and PerformanceInd. Eng. Chem. Res., 2014, 53 (5), pp 1916–1923.

• CRE for MAGIC (modular, agile, intensified & continuous) processes, 2015, Chemical Engineering Journal, (doi:10.1016/j.cej.2014.12.050)

• Selectivity engineering of the diazotization reaction in a continuous flow reactor c5re00056d

• Continuous flow nitration of o-Xylene: Effect of nitrating agent and feasibility of tubular reactors for scale-upDOI:10.1021/acs.oprd.5b00064, Org. Process Res. Dev. XXXX, XXX, XXX-XXX

• Discontinuous two step flow synthesis of m-aminoacetophenone; Green Process Synth; 3, 279-285

• Continuous flow nitration in miniaturized devices, Beilstein J. Org. Chem., 405-424

List of publications using AMaR reactors:

AMaR series flow reactors supplied with charging vessels, liquid metering pumps, heating cooling

circulators, back pressure regulator, condenser, gas liquid separator etc.

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Technical Specifications: Standard optional

Volume (ml) 1 ----

Flow rate (L/hr) 3.6 (for 1 sec. residence time) ----

Design Pressure (bar) 50 ----

Design Temperature (°C) -40 to 200 (with Viton ‘O’ ring) -40 to 250 (with Kalrez ‘O’ ring)

MOC SS 316 Hastelloy - B/C, Inconel, Monel, Titanium,

Tantalum lined, PTFE, CFT, PEEK

Heat transfer area (m²/m³) > 2000 ----

Dimensions (mm) 150 x 58 x 14 ----

End connections 3 nos. inlet & 1 no. outlet, 1/8” O/D 1/4-28 UNF connector

tube connector

Heating/ Cooling by dipping in thermostat SS304 jacket on either or both sides.

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AMaR-1: Micromixer (Patent filed)

Application: Mixing of miscible liquids or immiscible liquids or gases creating dispersion of immiscible fluids or gases in liquids and carrying out very fast, exothermic, homogeneous & heterogeneous reactions. Some of the tested applications include nitrations, halogenations, sulfoxidation, sulfonation, esterification, diazotization, condensation reactions, halogenations, reduction, oxidation, etc.

Technical Specifications: Standard Optional

Volume 1) 12 ml per plate

2) 50 ml per plate Upto 500 ml for 10 plates in series or parallel

3) 200 ml per plate Upto 2000 ml for 10 plates in series or parallel

Flow rate(L/hr) 0.144 to 24 (for single plate) 1.44 to 240 (for 10 plates in parallel)

Design Pressure(bar) 20 ----

Design Temperature(°C) -40 to 200 (with Viton ‘O’ ring) -40 to 250 (with Kalrez ‘O’ ring)

MOC SS316 Hastelloy B/C, Inconel, Monel, Titanium,

Tantalum Lined, PTFE,CFT , PEEK

Heat Transfer Area (m²/m³) > 2000 -----

End connections 3 nos Inlet & 1 No outlet Intermittent liquid addition or sampling

Heating/Cooling Circulating thermic fluid through

external SS304 jacket on both the sides -----

Upto 120 ml for 10 plates in series or parallel

AMaR-2: Microreactor(Patent filed)

Application: Mixing of miscible liquids or immiscible liquids or gases creating dispersion of immiscible fluids or gases in liquids and carrying out very fast, exothermic, homogeneous & heterogeneous reactions. Some of the tested applications include nitrations, halogenations, sulfoxidation, sulfonation, esterification, diazotization, condensation reactions, halogenations, reduction, oxidation etc.

Design: It comprises of broad converging diverging channel (with width to depth ratio between 5 to 20) with flow past triangular objects to avoid formation of dead zones. This helps to use maximum of the space and is scalable.

Flow pattern (AMaR-1 & 2)

Amar flow chemistry starter set one AmAR-1 reactor, two syringe pumps & one heating cooling bath circulator with skid.

Microwaveable AMaR-1 in PTFE/PEEK

Design: It comprises of broad channel (with width to depth ratio between 5 to20) with flow past triangular objects to avoid formation of dead zones. This helps to use maximum of the space and is scalable. Openable reactor plates enable easy cleaning especially for reactions involving solid formation. 12 ml AMaR-2

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Technical Specifications: Standard Optional

Volume (ml) 12, 30, 50, 100, 250, 500, 1000 ----

Flow rate (L/hr) 0.144 to 360 ----

Design Pressure (bar) 100 200/350

Design Temperature (°C) -40 to 250 500 (without jacket)

MOC SS 316 Hastelloy B/C, Inconel, Monel, Titanium,

Tantalum lined,

Heat transfer Area (m²/m³) 600 to 1800 ----

End connections 2 nos. inlet with Y mixture, 1 no. Intermittent addition or sampling ports,

outlet, pressure gauge, rupture disc safety relief valve, thermocouple

Heating/ Cooling Circulating thermic fluid through Heating Furnace

external SS304 jacket.

AMaR-3: Pilot scale 3D flow reactor

Application: Mixing of miscible liquids or immiscible liquids or gases creating dispersion of immiscible fluids or gases in liquids and carrying out very fast, exothermic, homogeneous, heterogeneous & catalytic hydrogenation reactions. Some of the tested applications include diazotization, nitrations, oxidation with different oxidizing agents, sulfoxidation, hydrogenation, sulfonation, etc. The reactor has been used in many industries for a wide range of reactions under various conditions from cryogenic to High temperature & High Pressure Reactions.

AMaR-3 A: Asymmetric AMaR-3

Application: Mixing of miscible liquids or immiscible liquids or gases creating dispersion of immiscible fluids or gases in liquids and carrying out very fast, exothermic, homogeneous, heterogeneous & catalytic hydrogenation reactions.

Other technical specifications: Same as AMaR-3

(Patent filed)

(Patent filed)

Design: It consists of a sequence of 3D converging units with or without obstructions. This is scalable and gives high throughput.

symmetric

Design: It consists of a sequence of a 3D converging units with or without obstructions. This is scalable and gives high throughput.

symmetric

Symmetric flow pattern Asymmetric flow pattern

1 ltr. AMaR-3 with flame proof pumps, control panel & control valvesExample: For an API or an intermediate with a product concentration of 20% in

the output stream, One (1) 36 lph reactor is needed to produce 50 metric tons/year.

36 lph % of product stream in the output streamper reactor 3 5 20 50 100

metric tons/year Number of reactors connected in parallel50 8 5 1 0 0

100 16 10 2 1 0250 24 6 2 1500 12 5 2

1000 10 52000 10

AMaR-3

30 ml AMaR-3

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Technical Specifications:

Volume (ml) 100, 250, 500, 1000, 2000

Flow rate (L/hr) 0.6 to 480

Design Pressure (bar) 50 (optional upto 350 bar)

Design Temperature (°C) -40 to 250

MOC SS 316, Optional: Hastelloy - B/C, Inconel, Monel, Titanium

Heat transfer Area (m²/m³) 600 to 1850

Heating/ Cooling Circulating thermic fluid through external MS / SS304 jacket

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Application: Mixing of miscible liquids or immiscible liquids or gases creating dispersion of immiscible fluids or gases in liquids and carrying out very fast, exothermic, homogeneous & heterogeneous reactions. The mass transfer will take place entirely depending upon the flow regime. This flow reactor has been fabricated and designed for various flow capacities for the industry. Standard as well as tailor made for each chemistry

Design: It consist of a sequence of coils made from pinched tube or normal tubes of various sizes. This is a scalable and high throughput flow reactor. The heat transfer area is high and the numbering up approach has been used for conducting the reactions. The reactor gives better mixing with several sampling ports measurement locations and flexibility to operate in parts.

AMaR-4 P: Tubular mixer / flow reactor(Patent filed)Application: miscible liquids or immiscible liquids or gases creating dispersion of immiscible fluids or gases in liquids and carrying out very fast, exothermic, homogeneous & heterogeneous reactions. Offers excellent mixing with no compromise on heat transfer rates. Can be used as a static mixer for homogeneous reaction for fluids of lower viscosity.

Excellent scalable flow reactor (pilot and production scale) for mixing of

AMaR-4: Production scale tubular flow reactor

Example: For an API or an intermediate with a product concentration of 20% in the output stream, One (1) 300 lph reactor is needed to produce 400 metric tons/year.

CSIR-NCL will help you customize AMaR-4 reactors specific to your reaction needsDesign and IP of this reactor design and different variations are owned by CSIR-NCL, Pune

AMaR-4480 lph % of product stream in the output stream

per reactor 3 5 20 50 100metric tons/year Number of reactors connected in parallel

100 1 1 0 0 0400 5 3 1 0 0

1200 9 2 1 02000 4 1 14000 3 1

Design: Helical pinch tubes of different sizes.

Flow pattern

Flow pattern

Technical specification same as above

The reactors like Amar4 are in successful operation in the industry for pilot and commercial scale production. Our clients have used them for producing fine and specialty chemicals involving immiscible phases for very exothermic reactions (- 40 kJ/mol<∆H < -210 kJ/mol) followed by their continuous quenching, extraction and work-up to the tube of 200 kg/day to 1800 kg/day. The pinched tube reactors are also used for carrying out pilot scale reactions, L-L extraction, G-L absorption, etc. These systems can be given any form to fit in the available space. Amar3 reactor has been successfully tested for G-L-S catalytic hydrogenation. The design of Amar2 helps to reduce the axial dispersion significantly and also eliminates dead zones in the reactor. This has helped for successfully replicating the lab scale results at pilot scale with no deviation in selectivity. All of these are scalable designs and we encourage our clients to use more number of similar reactors rather than using less number of large volume reactors. With our existing capabilities of designing fixed bed reactors we can even connect these flow reactors with fixed bed systems to facilitate multistep synthesis at various scales.

AMaR-4 with charging vessels, pumps & control panel

100 ml AMaR-4 P

2 ltr. AMaR-4

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Amar in collaboration with NCL is in continuous process of improving the existing reactors, designing and developing new reactors for the benefit of process industry.

AMaR-5: Solids handling flow reactor

APPLICATION: Suitable for application that generates solids during crystallization. Reaction involving slurries or the reactions where product or byproduct is solid (10% w/v and particle size <200 micron).

DESIGN: This reactor involves a passive technique using only the flow modifications without mechanical agitation or any external forces being applied apart from pumping. Internal geometry of the reactor helps to avoid retaining of solids generated in the flow.

Technical Specifications: Standard Optional

Volume (ml) 20, 50, 100, 250, 500, 1000 ----

Flow rate (L/hr) 0.24 to 360 ----

Design Pressure (bar) 20 100

Design Temperature (°C) -40 to 250 500

MOC SS 316 Hastelloy –B/C, Inconel, Monel, Titanium,

Tantalum

Heating/ Cooling Circulating thermic fluid Furnace heating

through external SS304 Jacket

AMaR-6: Catalytic mesh flow reactorApplication: Suitable for heterogeneous catalytic reactions like contact process, Haber Bosch process, Ostwald process, hydrogenation; Steam reforming, Ethylene oxide synthesis, Ziegler Natta Polymerization, hydrodesulphurization.

Technical Specifications: Standard Optional

Volume (ml) 10, 20, 50, 100 ----

Design Pressure (bar) 20 100

Design Temperature (°C) -40 to 250 500 (without jacket)

MOC SS 316 Hastelloy - B/C, Inconel, Monel, Titanium

End connections Inlet & outlet, 1/4” O/D tube 3/8” O/D tube connectors

connector

Heating/ Cooling Circulating thermic fluid Heating Furnace

through external SS304 jacket

Flow pattern

Type of particles Density Mass Particle size Flow rate Clogging

(gm/cc) (mm) (ml/min)

%

Glass particles (0.25 mm) 2.50 25 0.25 125 No clogging

Magnesium hydroxide 2.34 25 0.15 75 No clogging

Activated carbon 2-2.10 15 Fine powder 75 No clogging

Starch particles 0.82 8 1.10 75 No clogging

Crushed starch particles 0.82 10 0.55 75 Clogging in

the tube

from pump

Technical specifications

(Patent filed)

20 ml AMaR-5

150 ml AMaR-6

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They are used to accurately measure & control mass flow rate of gas (in gm/hr or LPH) & optionally totalized quantity of mass / volume (in gms / ltr.) charged in system at any point at high pressures up to 350 bar. The MFC assembly comes with inlet filter & check valve. MFC certified for use in zone 1 or zone 2 hazardous area offered on request.

Digital Pressure Indicator It consists of SS316 pressure sensor (transmitter) & digital pressure indicator/ controller with high pressure alarm & safety heater cutoff. Pressure sensors with Hastelloy C / PTFE / Inconel wetted parts can be offered on request.

Optional accessories are offered to increase the versatility of the equipment, to add value & feature to the standard product & to provide complete range of instrument/ equipment required for a particular application.

Pressure Sensor

Optional Accessories

Thermal Gas Mass Flow Controller (MFC)

To manually charge gases at constant desired pressures upto 350 bar / 5000 psi into the system. It comes with inlet - outlet pressure gauges, inline filters, check valves, On/Off valves etc.

Forward Gas Pressure Regulator

MFC

Flow Indicator & Totaliser

Ex-proof MFC

PTFE Pressure Sensor upto 15 bar

Safety rupture discs can be provided for pressure ratings ≥100 bar & pressure safety valves can be provided for any pressures from 1 to 350 bar with provision to vary release pressure within a certain range. These valves come with PTFE / Viton / Kalrez 'O' rings.

Pressure Safety Valve & Safety Rupture Disc

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Rupture Disc

Pressure Safety Valve

This system is used to charge the liquid at desired rate from as low as 0.6ml/hr. to 100Ltr./hr, when the system is under pressurized condition. The system comes with metering pump, flow indicator, controller, liquid charging vessel with optional heater, level indicator & weighing balance, pressure gauge, filter. Optionally pressure safety valve, flow totalizer is also provided. AMAR offers following types of pumps.

a) Low cost diaphragm metering pumps for pressures upto 100 bar & min. flow range of 0.1-1 lit/hr. to max. 10-100 lit/hr. The flow rates are varied by varying the motor speed with variable frequency drive. MOC: SS316, Hastelloy C, Titanium.

b) High pressure accurate HPLC low flow metering pumps for pressures upto 350 bar & flow range from 0.01 upto 100ml/min. MOC: SS316, PEEK, Hastelloy C & Titanium

c) Peristaltic pumps for low pressures

d) Low pressure low flow syringe pump

e) High pressure syringe pump for pumping slurry under pressures upto 350 bar

f) PTFE wetted parts diaphragm pump upto 10 bar

g) High pressure low flow gear pumps for pulseless flow

Optionally, in line coriolis flow meters with PID controllers & control valves can be connected to measure & control flow of the liquids accurately

Liquid Metering Pump System

(b)(a)

(d)

(f)

(e)

(c)

To measure precise amount/quantities of feed / product consumed or produced during process.

Weighing Balance

Cabinet with nitrogen purging for explosion proof zones can be offered by mounting nonexplosion proof instruments & assembly inside the cabinet

Purge Cabinet

(g)

Coriolis Mass Flow Controller

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Heating & Cooling Circulators

These are available either in bath system upto -75 °C to 200°C or single fluid closed loop system for

-60°C to 250°C for external circulation to heat or cool the load to desired temperature conditions. Only heating or only cooling system & chillers are also available.

Optional: Flexible insulated hose & suitable thermic fluid.

It is mounted on the vent line of the system & is used for maintaining constant pressure on the upstream. The pressure is maintained by releasing the excess pressure of gas / liquid.

Back Pressure Regulator (BPR)

Condenser

It is a SS-316 tube in tube out, helical coil in a vessel or reverse flow shell & tube heat exchanger for condensing the vent vapours from the system. It can be offered in all different MOC, higher pressure & different surface areas. The condensate can be collected separately in receiver .

It is a SS 316 pot connected at the outlet of the condensor to separate gas & liquid. It is offered in different volumes & MOC on request. It can be optionally provided with level indication & control.

Gas Liquid Separator

SCADA Software for remote operation & Recording

SCADA is a supervisory control & data acquisition software with all controllers / indicators having RS485 modbus communication port or PLC & HMI / touch panel, for online display, set point changes & data logging of pressure, temperature, liquid / gas flow rate with totaliser, heater temperature, level, weight, etc. remotely from PC as well as locally from panel. It gives continuous online data logging at predefined variable time interval, online graphical representation as well as historical data & graphs on PC . RS 485-232 convertor & cable upto 10m or higher is also supplied.

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Level sensor mounted on GLS or receiver pot for continuous sampling with minimum pressure drop

Level Control

Types of BPR

a) Manual variable pressure BPR for pressures upto 350 bar. MOC: SS316, Hastelloy C, Inconel, PEEK etc. for low to high flow rates.

b)Pneumatically actuated electronic BPR: here the pressure is set digitally & can be released at preset rate, pressures upto 350 bar. MOC: SS316, Hastelloy C, Inconel etc., for low to high flow rates.

c) Manually operated low cost fixed pressure BPR with wetted parts of PEEK™, ETFE, Perfluoroelastomer, where the pressure is fixed with respect to the BPR cartridge for back pressures ranging from 5 to1,000psi (0.3 to 69 bar). Operating flow rate: 0.1 to 10mL/min. Same body can house different pressure BPR cartridges.

d)Diaphragm type air operated BPR - MOC: ETFE and PFA, pressure range 0-300 psi, flow rates 0-20ml/min

(a)(b)

(c)

(d)

(a) PEEK

Liquid-Liquid SeparatorThis unit is used to separate slug flow of two immiscible liquids used in biphasic reaction or two phases of an extraction flow. MOC: ETFE, PFA and PTFE, pressure 300 psi.

Wet Gas MeterWet gas meter is an analog instrument used to measure exhaust gas flow for gas mixer & is available in all flow rate ranges. It can give output for digital flow indication

Sample / Status / Steam Selector ValveThese valves have unique variety of connecting slots and ports arrangements. It allows multiple planes of ports, facilitating unique multiposition configurations useful for stream selection, column selection or trapping. Can be configured for use at temperatures up to 350°C or pressures up to 10,000 psi.

Oven / FurnaceThis can be used for various applications commonly where condensation is major issue during process. The complete assembly can be placed inside oven to avoid condensation or to maintain particular temperature throughout the process. Temperature rating: 200°C for oven & 500°C for furnace.

Serving Industry since 1974.AMAR EQUIPMENTS PVT. LTD.

6, Parmar Industrial Estate, Bail Bazaar, Kale Marg, Kurla (W), Mumbai - 400 070. India.

Tel: +91-22-25095001 / 25143142 • Fax: +91-22-25109565 • Website: www.amarequip.com

E-mail: microreactor@amarequip.com / sales@amarequip.com / export@amarequip.com

®

• High Pressure Autoclaves • Gas Induction Reactors • Glass Autoclaves • High Through-put Catalyst Screening System • Vapour Phase Reactors

• Fixed Bed Reactors • Microreactors • Supercritical Fluid System • Corrosion Testing System • Magnetic Couplings / Stirrers

• Heating & Cooling Circulators • Sparkler & Leaf Filters

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Some of our valued customers

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