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Sonochemical Reactions and Synthesis

Sonochemistry is the application of ultrasound to chemical reactions and processes. The mechanism causing sonochemical effects in liquids is the phenomenon of acoustic cavitation.

Hielscher ultrasonic laboratory and industrial devices are used in a wide range of sonochemical processes. Ultrasonic cavitation intensifies and speeds up chemical reactions such as synthesis and catalysis.

Sonochemical Reactions

The following sonochemical effects can be observed in chemical reactions and processes:

  • increase in reaction speed
  • increase in reaction output
  • more efficient energy usage
  • sonochemical methods for switching of reaction pathway
  • performance improvement of phase transfer catalysts
  • avoidance of phase transfer catalysts
  • use of crude or technical reagents
  • activation of metals and solids
  • increase in the reactivity of reagents or catalysts (click here to read more about ultrasonically assisted catalysis)
  • improvement of particle synthesis
  • coating of nanoparticles

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Ultrasonic homogeizers installed as cluster of 7x UIP1000hdT (7x 1kW)

7 ultrasonic homogenizers of the model UIP1000hdT (7x 1kW ultrasonic power) installed as cluster for sonochemical reactions on industrial scale.

Advantages of Ultrasonically Intensified Chemical Reactions

Ultrasonically promoted chemical reactions are an established technique of process intensification in the field of chemical synthesis and processing. By harnessing the power of ultrasound waves, these reactions offer numerous advantages over conventional methods, improving chemical catalysis and synthesis. Turbo-fast conversion rates, excellent yields, enhanced selectivity, improved energy efficiency and reduced environmental impact are the main advantages of sonochemical reactions.

The table blow shows some prominent advantages of ultrasonically-promoted reaction vs conventional chemical reactions:

 

Reaction Reaction Time
Conventional
Reaction Time
Ultrasonics
Yield
Conventional (%)
Yield
Ultrasonics (%)
Diels-Alder cyclization 35 h 3.5 h 77.9 97.3
Oxidation of indane to indane-1-one 3 h 3 h less than 27% 73%
Reduction of methoxyaminosilane no reaction 3 h 0% 100%
Epoxidation of long-chain unsaturated fatty esters 2 h 15 min 48% 92%
Oxidation of arylalkanes 4 h 4 h 12% 80%
Michael addition of nitroalkanes to monosubstituted α,β-unsaturated esters 2 days 2 h 85% 90%
Permanganate oxidation of 2-octanol 5 h 5 h 3% 93%
Synthesis of chalcones by CLaisen-Schmidt condensation 60 min 10 min 5% 76%
UIllmann coupling of 2-iodonitrobenzene 2 h 2h less tan 1.5% 70.4%
Reformatsky reaction 12h 30 min 50% 98%

Ultrasonic Cavitation in Liquids

Cavitation, that is the formation, growth, and implosive collapse of bubbles in a liquid. Cavitational collapse produces intense local heating (~5000 K), high pressures (~1000 atm), and enormous heating and cooling rates (>109 K/sec) and liquid jet streams (~400 km/h). (Suslick 1998)

Cavitation using the UIP1000hd:

This video shows ultrasonic / acoustic cavitation in water - generated by the Hielscher UIP1000. Ultrasonic cavitation is used for many liquid applications.

Ultrasonic Cavitation in Liquids using the UIP1000

Video Thumbnail

Cavitation bubbles are vacuum bubbles. The vacuum is created by a fast moving surface on one side and an inert liquid on the other. The resulting pressure differences serve to overcome the cohesion and adhesion forces within the liquid.

Cavitation can be produced in different ways, such as Venturi nozzles, high pressure nozzles, high velocity rotation, or ultrasonic transducers. In all those systems the input energy is transformed into friction, turbulences, waves and cavitation. The fraction of the input energy that is transformed into cavitation depends on several factors describing the movement of the cavitation generating equipment in the liquid.

The intensity of acceleration is one of the most important factors influencing the efficient transformation of energy into cavitation. Higher acceleration creates higher pressure differences. This in turn increases the probability of the creation of vacuum bubbles instead of the creation of waves propagating through the liquid. Thus, the higher the acceleration the higher is the fraction of the energy that is transformed into cavitation. In case of an ultrasonic transducer, the intensity of acceleration is described by the amplitude of oscillation.

Higher amplitudes result in a more effective creation of cavitation. The industrial devices of Hielscher Ultrasonics can create amplitudes of up to 115 µm. These high amplitudes allow for a high power transmission ratio what in turn allows to create high power densities of up to 100 W/cm³.

In addition to the intensity, the liquid should be accelerated in a way to create minimal losses in terms of turbulences, friction and wave generation. For this, the optimal way is a unilateral direction of movement.

Ultrasonication is known to improve transesterification reactions thereby giving e.g. higher methyl esters and polyols. Hielscher Ultrasonics manufactures industrial ultrasonic probes and reactors for high throughputs.

Ultrasonic reactor with 16,000 watts for sonochemically enhanced inline transesterification.

Ultrasound is used because of its effects in processes, such as:

  • preparation of activated metals by reduction of metal salts
  • generation of activated metals by sonication
  • sonochemical synthesis of particles by precipitation of metal (Fe, Cr, Mn, Co) oxides, e.g. for use as catalysts
  • impregnation of metals or metal halides on supports
  • preparation of activated metal solutions
  • reactions involving metals via in situ generated organoelement species
  • reactions involving non-metallic solids
  • crystallization and precipitation of metals, alloys, zeolithes and other solids
  • modification of surface morphology and particle size by high velocity interparticle collisions
    • formation of amorphous nanostructured materials, including high surface area transition metals, alloys, carbides, oxides and colloids
    • agglomeration of crystals
    • smoothing and removal of passivating oxide coating
    • micromanipulation (fractionation) of small particles
  • dispersion of solids
  • preparation of colloids (Ag, Au, Q-sized CdS)
  • intercalation of guest molecules into host inorganic layered solids
  • sonochemistry of polymers
    • degradation and modification of polymers
    • synthesis of polymers
  • sonolysis of organic pollutants in water

Sonochemical Equipment

Most of the mentioned sonochemical processes can be retrofitted to work inline. We will be glad to assist you in choosing the sonochemical equipment for your processing needs. For the research and for the testing of processes we recommend our laboratory devices or the UIP1000hdT set.

If required, FM and ATEX certified ultrasonic devices and reactors (e.g. UIP1000-Exd) are available for the sonication of flammable chemicals and product formulations in hazardous environments.

Ultrasonic Cavitation Changes Ring-Opening Reactions

Ultrasonication is an alternative mechanism to heat, pressure, light or electricity to initiate chemical reactions. Jeffrey S. Moore, Charles R. Hickenboth, and their team at the Chemistry Faculty at University of Illinois at Urbana-Champaign used ultrasonic power to trigger and manipulate ring-opening reactions. Under sonication, the chemical reactions generated products different from the the ones predicted by orbital symmetry rules (Nature 2007, 446, 423). The group linked mechanically sensitive 1,2-disubstituted benzocyclobutene isomers to two polyethylene glycol chains, applied ultrasonic energy, and analyzed the bulk solutions by using C13 nuclear magnetic resonance spectroscopy. The spectra showed that both the cis and trans isomers provide the same ring-opened product, the one expected from the trans isomer. While thermal energy causes random Brownian motion of the reactants, the mechanical energy of ultrasonication provides a direction to atomic motions. Therefore, cavitational effects efficiently direct the energy by straining the molecule, reshaping the potential energy surface.

Ultrasonication improves the bottom-up synthesis of nanoparticles.

Probe-type ultrasonicators as the UP400St intensify the synthesis of nanoparticles. The sonochemical route is simple, efficacious, rapid and works with non-toxic chemicals under mild conditions.

High Performance Ultrasonicators for Sonochemistry

Hielscher Ultrasonics supplies ultrasonic processors for lab and industry. All Hielscher ultrasonicators are very powerful and robust ultrasound machines and built for continuous 24/7 operation under full load. Digital control, programmable settings, temperature monitoring, automatic data protocolling and remote browser control are just a few features of Hielscher ultrasonicators. Designed for high performance and comfortable operation, users value the safe and easy handling of Hielscher Ultrasonics equipment. Hielscher industrial ultrasonic processors deliver amplitudes of up to 200µm and are ideal for heavy duty applications. For even higher amplitudes, customized ultrasonic sonotrodes are available.
The table below gives you an indication of the approximate processing capacity of our ultrasonicators:

Batch Volume Flow Rate Recommended Devices
1 to 500mL 10 to 200mL/min UP100H
10 to 2000mL 20 to 400mL/min UP200Ht, UP400St
0.1 to 20L 0.2 to 4L/min UIP2000hdT
10 to 100L 2 to 10L/min UIP4000hdT
n.a. 10 to 100L/min UIP16000
n.a. larger cluster of UIP16000

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Ultrasonic high-shear homogenizers are used in lab, bench-top, pilot and industrial processing.

Hielscher Ultrasonics manufactures high-performance ultrasonic homogenizers for mixing applications, dispersion, emulsification and extraction on lab, pilot and industrial scale.



Literature / References


High performance ultrasonics! Hielscher's product range covers the full spectrum from the compact lab ultrasonicator over bench-top units to full-industrial ultrasonic systems.

Hielscher Ultrasonics manufactures high-performance ultrasonic homogenizers from lab to industrial size.

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