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U lt r a - p u r e c h e m i c a l s p r o d u c t i o n us i n g t h e TNO H y d r au l i c Wa s h C o l u m n ( TNO H W C ® )

Melt crystallization

Melt crystallization is a valuable tool in your company for the production


of ultra pure chemicals (well over 99.9% purity). TNO has developed the
TNO HWC® for crystallization from the melt. This proprietary technology
provides opportunities for producing ultra pure chemicals on a large
scale with a low consumption of energy, without using solvents.

Main features of interest to the This enables the use of extra purification
Chemical Industry methods around the melting temperature,
• Single step process usually combines like washing with the pure melts,
high purity (> 99.9%) with high sweating, etc. In general terms, it may be
recovery. said that melt crystallization’s energy
– Low energy consumption. requirement, in principle, is low. The heat
• No solvent. of transition in crystallization is typically
• Continuous operation. two to five times lower than in distillation.
Moreover, the need of reflux is limited
The merits of melt due to the high purification efficiency.
crystallization Melt crystallization is often superior on
Melt crystallization differs from other an economic level as well as from an
crystallization methods in the fact that environmental point of view for ultra The TNO demonstration wash column operating
the operating temperature is close to the purification and separation of isomers with para-Xylene. The separation effect is
visualized by addition of a dye to the mixture.
melting temperature of the main compared to other typical separation
component. operations like distillation, adsorption

104526_TNO_melt_cryst.indd 1 5/25/11 9:00:18 AM


C h e m i c a l p r o c e s s t ec h n o lo gy f o r e f f i c i e n t p r o d u c t i o n

filtrate (residue) washing and the re-crystallization of


wash liquid at the wash front cause a
filtrate recirculation
settling zone very good purification result. The three
zones – feed suspension, unwashed and
washed bed – are clearly visible in the
slurry feed
photograph above.
Melt crystallization is especially
Solid-liquid separation
interesting for low molecular weight
organic feed mixtures (molecular weight
bed level
< 200 g/mol) with a melting point
crystal bed between –50 and 200 °C. Next to 15
bulk scale applications up to 200 fine
porous filter
organic chemicals have been identified
filter tube which can be purified with this
wash front technology.
product valve (pressure control valve) Beside purification of organic chemicals,
Countercurrent washing this technique is also suited for
with pure melt
purification of inorganic materials (e.g.
product
rotating knife (pure molten crystals) phosphoric acid, hydrogen peroxide) and
metals (e.g. aluminium).

melter
Schematic diagram of the TNO wash column

and absorption. Furthermore, the use of consumed during washing (internal


an organic solvent is avoided, which will recycle).
have a positive impact on safety and the Typically the wash column product will
environment and on application in food contain 100-1000 times less impurity
industry. Due to the relatively low molecules than the impure mother liquor
operating temperature compared with from which the crystals were grown.
distillation, this process is often
applicable. Survey of organic compounds of interest
successfully investigated at TNO
TNO hydraulic wash column Acetonitril para-Chloronitrobenzene
When cooling a melt below the Acrylic acid para-Chloronitrobenzene
crystallization temperature in general Caprolactam para-Dichlorobenzene
relatively pure crystals will be formed, Maleic anhydride para-Xylene TNO
because the impurities with their Napthalene Phenol Leeghwaterstraat 46
deviating size and/or shape will not fit in 2628 CA Delft
the highly structured crystal lattice. In Process description The Netherlands
order to benefit from the high intrinsic The TNO hydraulic wash column consists
purity of the crystals, these need to be of a cylinder, in which a number of filter P.O. Box 155
separated almost completely from the tubes of a constant diameter extend in 2600 AD Delft
impure mother liquor which contains axial direction. The wash column is fed The Netherlands
most of the impurities. A TNO hydraulic with the suspension from a melt
wash column is perfectly suited for that crystallizer. The mother liquor escapes Dr. Jean-Marie Bassett
task since it combines continuous solid via filters. The filters retain the crystals Business Development Manager
– liquid separation with a highly efficient and a packed bed of crystals is formed Chemicals Sector
counter current washing operation. The within the cylinder. The bed is T +31 88 866 8118
wash liquid is usually a small part of the transported downwards by means of M +31 6 104 804 73
pure molten crystals and it is not hydraulic pressure as the filtrate flows Jean-marie.bassett@tno.nl
toward the filters. The bed is
TNO wash column concept offers disintegrated at the bottom of the column Martijn de Graaff MSc.
• A straight forward scale up strategy. and the crystals are suspended in the Business Development Manager
• A broad turn down ratio. circulating melt and then tapped off as Sustainable Chemical Industry
• Control strategies for automatic molten product. A part of the molten T +31 88 866 6437
operation. product is forced through the packed M +31 6 222 608 71
• High specific throughput up to 15 ton/hr crystal bed and re-crystallizes on the martijn.degraaff@tno.nl
per m2 cross sectional area. colder crystals thereby producing the
• Low operating costs. socalled wash front. The counter-current www.tno.nl

104526_TNO_melt_cryst.indd 2 5/25/11 9:00:18 AM