IceCube™ Flow Reactor - Safe Exothermic Reactions Made Easy

Low temperature continuous flow reactor for high energy reactions

The IceCube™ is a revolutionary continuous flow low temperature reactor specifically for high energy reactions to be performed in a highly controlled and safe manner. The system is made up of 3 modules. The Ozone Module, Pump Module, and Reactor Module. The modules can be configured or purchased separately to match the configuration you want.

Ozone Module gives you a safe and efficient way of generating ozone from oxygen. The ozone/oxygen amount is precisely controlled through the built-in mass flow controller. The system can also be used as a powerful and compact stand alone ozonizer.

Oxygen flow rate: 10-100 mL/min.
O3/O2 v/v%: 14% at 20 mL/min oxygen flow rate.

Reactor Module is a highly versatile reactor capable of controlling even extremely exothermic reactions safely and simply. Composed of two reactor plates with Peltier heating/cooling, and a reaction line made of Teflon for wide chemical compatibility. The system may be configured for 2, 3, or 4 reactants in 1 sequence. Difficult or dangerous reactions such as lithiation, azide generation or ozonolysis may now be performed and quenched immediately without the need for isolation of dangerous intermediates.

Main reactor block temp -70 – +80°C
Maximum main reactor volume 8 mL
Tubing 1/16” OD 1mm ID PTFE
Maximum precooler volume 4 mL
Quench reactor block temp. -30 – +80°C
Quench reactor volume 4 mL
Number of mixers 2
Pressure capability up to 6 bar

Pump Module is made up of 2 rotary piston pumps, which have good chemical compatibility. The pumps are connected two 3-way valves, which control the path of reactant or solvent through the reactor. Multiple pump modules can be purchased. Single pumps also. Flow rate: 0.2 – 4 mL/min

Reactions such as lithiation, ozonolysis and nitration can now be performed in any lab, by any chemist, therefore there is no need to avoid or work around these normally hazardous reactions. Also, the unstable intermediates that are required for exothermic reactions to have a high yield and conversion require a firm control over parameters such as temperature and pressure, which are problematic in traditional batch synthesis techniques, therefore their utilization is limited. With the IceCube™ flow reactors’ high heat and mass transfer capability, chemists can exploit these previously untapped or avoided chemistries.


Swern Oxidation

Swern oxidation with IceCube Flow Reactor

Nitration

Nitration Reaction with IceCube flow reactor

Lithiation

Lithiation with IceCube flow reactor

Ozonolysis

Features

Safe

  • High energy reactions can now be performed in an extremely safe and controlled manner through excellent temperature control.
  • Two reactors are connected in sequence, so any hazardous intermediate generated in the first reactor can be immediately reacted without need for isolation.
  • Automatic blockage/leakage detection.
  • Any excess Ozone generated is consumed using a quench flask.
  • High chemical resistance allowing the use of different reagent, even strong acids.

Simple

  • Everything is software controlled. Just set few parameters, press “Start”, and let the IceCube™ to do the rest.
  • Intuitive software control
  • Chemistry application focused design
  • Only tap water needed for cooling

Versatility

  • Wide temperature range; from -70°C - +80°C
  • Two reactor blocks for multi step reactions
  • Modular system
  • Only buy and use the modules you need

High Control

  • Built in safety feature, such as automatic stop features in case of alarm
  • Continuous real time feedback from the control unit

Innovative

  • Makes dangerous exothermic reactions safe to do
  • Generate libraries from previously forbidden chemistries with upcoming automation system

Selective

  • Precooling before mixer, so reaction does not start immediately at RT
  • Mixing under cooled environment
  • Changeable reaction temperature in both reaction zones
  • Fast response to temperature change to avoid generation of side product

Productivity

  • Easy scale-up from mg to kilo scale

FAQ

What is the basic set up of the system?
The general setting up contains 4 main parts:
........ Dual pump system
........ Ozone Module
........ Reactor module
........ Control unit

Can I use more pumps?
Yes, and it can be controlled by the control unit as well.

Are there any preferred configurations?
By default the control unit provides you the following predefined configuration:
........ Ozonolysis (2 pumps are used and the Ozone Module)
........ 2 pumps 1 reactor zone (2 pumps and the main reactor zone are in use)
........ 3 pumps 2 reactor zones (3 pumps and both reactor zones are in use)

Can I add my own configurations?
Yes, you can built in your own configuration in the software.

How easy is it to make the system ready physically for these configurations e.g. change from mixture of 2 liquids to mixing liquid with ozone for ozonolysis?
You only need to include a mixer and other Teflon tubing to supply either a liquid or a gas, which takes only a few minutes to do.

What happens if I get a blockage?
Standard Teflon tubing is utilized, so this may be cheaply replaced using a pair of scissors instead of having to buy a new expensive glass reactor.

How can you vary the reaction zone for scaling up?
You can change to another reaction volume easily in seconds. The length or internal diameter of the reaction line may be changed by swapping over reactor plates.

What does the reaction area look like?
You can use either 1/8” or 1/16” Teflon tubes embedded in a plate. The plate has grooves so changing the coil takes only few minutes and is much cheaper than buying a new chip reactor.

What solvents can be used?
All the wetted parts of the system is made of Teflon, which can tolerate even strong acids.

Can I perform reactions require inert conditions?
Yes, e.g. lithiation where the BuLi require inert atmosphere has been already successfully run.

Can you react other gases to perform different reactions?
You can introduce other gases to perform e.g. oxidation under pressure up to 6 bar.

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