Hielscher Ultrasound Technology

Ultrasonic Saponification

  • Saponification is a widely used chemical reaction to produce soap from oils or fats and a base.
  • Ultrasonication intensifies the saponification reaction, which results in a faster reaction and a more complete conversion.
  • By avoiding the excessive use of catalyst and being an energy-efficient processing method, sonication is an environmental-friendly processing technique.

Ultrasonically Promoted Saponification

Saponification is at the chemical process of soap making. It is the reaction in which the raw material of fats or oils (triglycerides) react with an alkali reactant in order to form soap. Ultrasonication promotes the phase transfer catalysis resulting in increased reaction speed, more complete conversion and avoids the excessive use of base reagents such as potassium hydroxide (KOH) or sodium hydroxide (NaOH). The ultrasonically initiated alkaline hydrolysis can be easily implemented in commercial soap manufacturing to produce higher output in shorter time without using any catalyst or reducing the amounts of catalyst used.

The Advantages of Ultrasonic Saponification

  • Faster reaction
  • Higher conversion
  • No excessive use of base reagents
  • No excessive use of catalyst
  • More complete reaction
  • Green process

Case Studies of Ultrasonic Saponification

Various research studies have shown that sonication promotes the saponification of triglycerides into soap. Ultrasonic saponification accelerates and increases the conversion whilst saving or avoiding the use of catalyst. This makes ultrasonic saponification a highly efficient production method.

UIP2000hdT - 2kW ultrasonicator for liquid processing.

UIP2000hdT (2kW) for saponification

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Ultrasonic Initiation of the Alkaline Hydrolysis of Triglycerides (Saponification) Without Phase Catalyst

UP400St Ultrasonic Homogenizer 400 watts for batch sonicationMercantili et al. (2013) studied the effects of ultrasonication on the alkaline hydrolysis of triglycerides, known as saponification. They used sonication to initiate the alkaline hydrolysis of sunflower oil. Potassium hydroxide (KOH) was used as alkali base. It was shown that ultrasound is effective as a power source to initiate and drive the reaction, that a high reaction yield is achievable in only 15 min of total power application while working at ambient temperature, and that no detectable by‐products are generated during the reaction. The comparison of an ultrasonic bath and a probe-type ultrasonocator shows the ultrasonic probe to be the superior technique. The study demonstrates that ultrasonic saponification yields in a good conversion without the need for excess alkali or phase transfer catalysis.

Ultrasonic saponification is a green sonochemical process that accelerates the reaction and improves the conversion.

Alkaline hydrolysis of triacylglycerol

Ultrasonically Promoted Phase Transfer Reaction for Saponification

Bhatkhande et al. (1998) showed that sonication of vegetable oils such as soybean oil could be efficiently saponified using aqueous KOH and different PTCs at room temperature. The extent of saponification was studied using the saponification value as a reference. Optimizations of various parameters such as time, selection of phase transfer catalysts, quantity of catalyst used, quantity of KOH and quantity of water were carried out using sonication and stirring. To study the effect of ultrasound, the saponification was also carried out at 35ºC under different conditions, namely stirring, sonication, stirring and sonication, and heating at 100ºC. It was found that the heterogeneous liquid-liquid phase saponification of different vegetable oils using aqueous KOH/CTAB was significantly accelerated at 35ºC under sonication and stirring.

High Performance Ultrasonicators

Hielscher Ultrasonics supplies high-performance ultrasonic equipment for lab, pilot and industrial production. The robust and reliable ultrasonicators are used for various sonochemical reactions such as saponification. Hielscher’s probe-type ultrasonicators can be used in batch and inline mode. All important process parameters – amplitude, pressure, temperature – can be precisely controlled and ensure reproducible results.
Colored touch display of the new hdT series of Hielscher's industrial ultrasonicatorsThe digital control automatically records the process parameters and store them on the integrated SD-card. Pre-settings and remote browser control make the sonication process very simple and user-friendly.
For many sonochemical reactions a certain temperature must be maintained, so temperature control is important. Hielscher’s digital ultrasonicators come with a thermo-couple and temperature control. Jacketed flow cell allow for heat dissipation.
The robustness of Hielscher’s ultrasonic equipment allows for 24/7 operation at heavy duty and in demanding environments.
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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Hielscher Ultrasonics manufactures high-performance ultrasonicators for sonochemical applications.

High-power ultrasonic processors from lab to pilot and industrial scale.

Literature/References

  • Bhatkhande, B.S.; Samant, Shriniwas D. (1998): Ultrasound assisted PTC catalyzed saponification of vegetable oils using aqueous alkali. Ultrasonics Sonochemistry Vol. 5, Issue 1, 1998. 7-12.
  • Mercantili, Laura; Séamus, Frank Davis; Higson, P. J. (2014): Ultrasonic Initiation of the Alkaline Hydrolysis of Triglycerides (Saponification) Without Phase Catalysis. Journal of Surfactant and Detergents Vol. 17, Isssue 1, Jan 2014. 133-141.


Facts Worth Knowing

Sonochemistry

Power ultrasound is applied to chemical processes such as synthesis and catalysis (also called sono-synthesis and sono-catalysis, respectively) in order to initiate and intensify the reaction. Various applications of ultrasonic irradiation in organic synthesis have been in depth investigated and developed for industrial production. Sonochemical treatments can increase the rate of reaction, yield and selectivity of desired products under significantly milder condition. This makes the ultrasonic treatment an effective and environmental-friendly processing technique. Ultrasonically assisted phase transfer catalysis (PTC) is proven to be a drastically more efficient and effective method for organic reactions compared to the same reaction at silence condition. For example, the Cannizarro reaction catalyzed by an ultrasonically-assisted phase transfer catalysis is significantly sped up resulting in a rapid conversion. Another prominent example is the transesterification of triglycerides (i.e. vegetable oils, animal fats) and methanol in presence of KOH as catalyst and power ultrasound. The ultrasonic transesterification yields in high-quality biodiesel produced in a rapid conversion and a very efficient, economical process.

Ultrasonic / acoustic cavitation creates highly intense forces which opens the cell walls known as lysis (Click to enlarge!)

Ultrasonic extraction is based on acoustic cavitation and its hydrodynamic shear forces

Saponification

Saponification describes the chemical reaction that produces soap. In the saponification process, vegetable oils or animal fats are converted into fatty acid salts – the “soap” – and glycerol, which is an alcohol. The reaction requires a solution of an alkali base (e.g., NaOH or KOH) in water and also heat to initiate the reaction.
The reaction steps of saponification are the following:

  1. Nucleophilic attack of the fatty acid esters by the hydroxide
  2. Leaving group removal
  3. Deprotonation

The saponification reaction is used commercially to produce soaps and lubricants.
While sodium hydroxide hard soap and potassium hydroxide soft soap are used for everyday cleaning, there are also special soaps produced using other metal hydroxides. For example, lithium soaps and calcium soaps are used as lubricating greases. There are also “complex soaps” consisting of a mixture of metallic soaps.

Hydrolysis

Hydrolysis involves the reaction of an organic chemical with water to form two or more new substances and usually means the cleavage of chemical bonds by the addition of water. Esters can be cleaved back into a carboxylic acid and an alcohol by reaction with water and a base. Soap is produced by the hydrolysis of the esters of fat or oil.

Alkaline Base

Alkaline base reactants (lyes) are required for the saponification of oils and fats. The triglycerides are reacted with a base – sodium or potassium hydroxide – in order to produce glycerol and a fatty acid salt, the so-called “soap”. Potassium hydroxide is an inorganic compound with the formula KOH, and is commonly called caustic potash. Sodium hydroxide (NaOH) is another prototypical strong base. When sodium hydroxide is used, a hard soap is produced, whilst the use of potassium hydroxide results in a soft soap.

Reactant vs Reagent

A reactant is a substance that is used up or consumed in a chemical reaction. In comparison to a reagent, a reactant is required in larger amounts. A reagent is a substance that is used to initiate a reaction, to support the reaction and is consumed in a reaction, in contrasts to catalysts which are not consumed in a reaction.