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Fractional crystallization (chemistry) - Wikipedia
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class="interlanguage-link-target"><span>العربية</span></a></li><li class="interlanguage-link interwiki-ca mw-list-item"><a href="https://ca.wikipedia.org/wiki/Cristal%C2%B7litzaci%C3%B3_fraccionada" title="Cristal·lització fraccionada – Catalan" lang="ca" hreflang="ca" data-title="Cristal·lització fraccionada" data-language-autonym="Català" data-language-local-name="Catalan" class="interlanguage-link-target"><span>Català</span></a></li><li class="interlanguage-link interwiki-cs mw-list-item"><a href="https://cs.wikipedia.org/wiki/Frak%C4%8Dn%C3%AD_krystalizace_(chemie)" title="Frakční krystalizace (chemie) – Czech" lang="cs" hreflang="cs" data-title="Frakční krystalizace (chemie)" data-language-autonym="Čeština" data-language-local-name="Czech" class="interlanguage-link-target"><span>Čeština</span></a></li><li class="interlanguage-link interwiki-de mw-list-item"><a href="https://de.wikipedia.org/wiki/Fraktionierte_Kristallisation_(Chemie)" title="Fraktionierte Kristallisation (Chemie) – German" lang="de" hreflang="de" data-title="Fraktionierte Kristallisation (Chemie)" data-language-autonym="Deutsch" data-language-local-name="German" class="interlanguage-link-target"><span>Deutsch</span></a></li><li class="interlanguage-link interwiki-eo mw-list-item"><a href="https://eo.wikipedia.org/wiki/Frakcia_kristaligo_(kemio)" title="Frakcia kristaligo (kemio) – Esperanto" lang="eo" hreflang="eo" data-title="Frakcia kristaligo (kemio)" data-language-autonym="Esperanto" data-language-local-name="Esperanto" class="interlanguage-link-target"><span>Esperanto</span></a></li><li class="interlanguage-link interwiki-fr mw-list-item"><a href="https://fr.wikipedia.org/wiki/Cristallisation_fractionn%C3%A9e_(chimie)" title="Cristallisation fractionnée (chimie) – French" lang="fr" hreflang="fr" data-title="Cristallisation fractionnée (chimie)" data-language-autonym="Français" data-language-local-name="French" class="interlanguage-link-target"><span>Français</span></a></li><li class="interlanguage-link interwiki-hy mw-list-item"><a href="https://hy.wikipedia.org/wiki/%D4%BF%D5%B8%D5%BF%D5%B8%D6%80%D5%A1%D5%AF%D5%A1%D5%B5%D5%AB%D5%B6_%D5%A2%D5%B5%D5%B8%D6%82%D6%80%D5%A5%D5%B2%D5%A1%D6%81%D5%B8%D6%82%D5%B4" title="Կոտորակային բյուրեղացում – Armenian" lang="hy" hreflang="hy" data-title="Կոտորակային բյուրեղացում" data-language-autonym="Հայերեն" data-language-local-name="Armenian" class="interlanguage-link-target"><span>Հայերեն</span></a></li><li class="interlanguage-link interwiki-id mw-list-item"><a href="https://id.wikipedia.org/wiki/Kristalisasi_fraksional_(kimia)" title="Kristalisasi fraksional (kimia) – Indonesian" lang="id" hreflang="id" data-title="Kristalisasi fraksional (kimia)" data-language-autonym="Bahasa Indonesia" data-language-local-name="Indonesian" class="interlanguage-link-target"><span>Bahasa Indonesia</span></a></li><li class="interlanguage-link interwiki-ja mw-list-item"><a href="https://ja.wikipedia.org/wiki/%E5%88%86%E5%88%A5%E6%99%B6%E6%9E%90%E6%B3%95" title="分別晶析法 – Japanese" lang="ja" hreflang="ja" data-title="分別晶析法" data-language-autonym="日本語" data-language-local-name="Japanese" class="interlanguage-link-target"><span>日本語</span></a></li><li class="interlanguage-link interwiki-pt mw-list-item"><a href="https://pt.wikipedia.org/wiki/Cristaliza%C3%A7%C3%A3o_fracionada_(qu%C3%ADmica)" title="Cristalização fracionada (química) – Portuguese" lang="pt" hreflang="pt" data-title="Cristalização fracionada (química)" data-language-autonym="Português" data-language-local-name="Portuguese" class="interlanguage-link-target"><span>Português</span></a></li><li class="interlanguage-link interwiki-sl mw-list-item"><a href="https://sl.wikipedia.org/wiki/Frakcionirana_kristalizacija_(kemija)" title="Frakcionirana kristalizacija (kemija) – Slovenian" lang="sl" hreflang="sl" data-title="Frakcionirana kristalizacija (kemija)" data-language-autonym="Slovenščina" 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(prefers-color-scheme:dark){html.skin-theme-clientpref-os .mw-parser-output .infobox-full-data:not(.notheme) div:not(.notheme){background:#1f1f23!important;color:#f8f9fa}}@media(min-width:640px){body.skin--responsive .mw-parser-output .infobox-table{display:table!important}body.skin--responsive .mw-parser-output .infobox-table>caption{display:table-caption!important}body.skin--responsive .mw-parser-output .infobox-table>tbody{display:table-row-group}body.skin--responsive .mw-parser-output .infobox-table tr{display:table-row!important}body.skin--responsive .mw-parser-output .infobox-table th,body.skin--responsive .mw-parser-output .infobox-table td{padding-left:inherit;padding-right:inherit}}</style><table class="infobox hlist" style="width:18em; text-align:center; font-size:95%;"><tbody><tr><th colspan="2" class="infobox-above" style="padding-bottom:0.3em; background:transparent; line-height:1.1em; font-size:125%; font-weight:bold;"><a href="/wiki/Crystallization" title="Crystallization">Crystallization</a></th></tr><tr><td colspan="2" class="infobox-image"><span class="mw-default-size" typeof="mw:File"><a href="/wiki/File:Process-of-Crystallization-200px.png" class="mw-file-description"><img src="//upload.wikimedia.org/wikipedia/commons/c/ce/Process-of-Crystallization-200px.png" decoding="async" width="200" height="74" class="mw-file-element" data-file-width="200" data-file-height="74" /></a></span></td></tr><tr><th colspan="2" class="infobox-header" style="background:#E7C6A5;">Fundamentals</th></tr><tr><td colspan="2" class="infobox-full-data" style="line-height:1.4em;"> <ul><li><a href="/wiki/Crystal" title="Crystal">Crystal</a></li> <li><a href="/wiki/Crystal_structure" title="Crystal structure">Crystal structure</a></li> <li><a href="/wiki/Nucleation" title="Nucleation">Nucleation</a></li></ul> </td></tr><tr><th colspan="2" class="infobox-header" style="background:#E7C6A5;">Concepts</th></tr><tr><td colspan="2" class="infobox-full-data" style="line-height:1.4em;"> <ul><li><a href="/wiki/Crystallization" title="Crystallization">Crystallization</a></li> <li><a href="/wiki/Crystal_growth" title="Crystal growth">Crystal growth</a></li> <li><a href="/wiki/Recrystallization_(chemistry)" title="Recrystallization (chemistry)">Recrystallization</a></li> <li><a href="/wiki/Seed_crystal" title="Seed crystal">Seed crystal</a></li> <li><a href="/wiki/Protocrystalline" title="Protocrystalline">Protocrystalline</a></li> <li><a href="/wiki/Single_crystal" title="Single crystal">Single crystal</a></li></ul> </td></tr><tr><th colspan="2" class="infobox-header" style="background:#E7C6A5;">Methods and technology</th></tr><tr><td colspan="2" class="infobox-full-data" style="line-height:1.4em;"> <ul><li><a href="/wiki/Boule_(crystal)" title="Boule (crystal)">Boules</a></li> <li><a href="/wiki/Bridgman%E2%80%93Stockbarger_method" title="Bridgman–Stockbarger method">Bridgman–Stockbarger method</a></li> <li><a href="/wiki/Van_Arkel%E2%80%93de_Boer_process" title="Van Arkel–de Boer process">Van Arkel–de Boer process</a></li> <li><a href="/wiki/Czochralski_method" title="Czochralski method">Czochralski method</a></li> <li><a href="/wiki/Epitaxy" title="Epitaxy">Epitaxy</a></li> <li><a href="/wiki/Flux_method" title="Flux method">Flux method</a></li> <li><a class="mw-selflink selflink">Fractional crystallization</a></li> <li><a href="/wiki/Fractional_freezing" title="Fractional freezing">Fractional freezing</a></li> <li><a href="/wiki/Hydrothermal_synthesis" title="Hydrothermal synthesis">Hydrothermal synthesis</a></li> <li><a href="/wiki/Kyropoulos_method" title="Kyropoulos method">Kyropoulos method</a></li> <li><a href="/wiki/Laser-heated_pedestal_growth" title="Laser-heated pedestal growth">Laser-heated pedestal growth</a></li> <li><a href="/wiki/Micro-pulling-down" title="Micro-pulling-down">Micro-pulling-down</a></li> <li><a href="/wiki/Shaping_processes_in_crystal_growth" title="Shaping processes in crystal growth">Shaping processes in crystal growth</a></li> <li><a href="/wiki/Skull_crucible" title="Skull crucible">Skull crucible</a></li> <li><a href="/wiki/Verneuil_method" title="Verneuil method">Verneuil method</a></li> <li><a href="/wiki/Zone_melting" title="Zone melting">Zone melting</a></li></ul> </td></tr><tr><td colspan="2" class="infobox-navbar"><link rel="mw-deduplicated-inline-style" href="mw-data:TemplateStyles:r1129693374"><style data-mw-deduplicate="TemplateStyles:r1239400231">.mw-parser-output .navbar{display:inline;font-size:88%;font-weight:normal}.mw-parser-output .navbar-collapse{float:left;text-align:left}.mw-parser-output .navbar-boxtext{word-spacing:0}.mw-parser-output .navbar ul{display:inline-block;white-space:nowrap;line-height:inherit}.mw-parser-output .navbar-brackets::before{margin-right:-0.125em;content:"[ "}.mw-parser-output .navbar-brackets::after{margin-left:-0.125em;content:" ]"}.mw-parser-output .navbar li{word-spacing:-0.125em}.mw-parser-output .navbar a>span,.mw-parser-output .navbar a>abbr{text-decoration:inherit}.mw-parser-output .navbar-mini abbr{font-variant:small-caps;border-bottom:none;text-decoration:none;cursor:inherit}.mw-parser-output .navbar-ct-full{font-size:114%;margin:0 7em}.mw-parser-output .navbar-ct-mini{font-size:114%;margin:0 4em}html.skin-theme-clientpref-night .mw-parser-output .navbar li a abbr{color:var(--color-base)!important}@media(prefers-color-scheme:dark){html.skin-theme-clientpref-os .mw-parser-output .navbar li a abbr{color:var(--color-base)!important}}@media print{.mw-parser-output .navbar{display:none!important}}</style><div class="navbar plainlinks hlist navbar-mini"><ul><li class="nv-view"><a href="/wiki/Template:Crystallization" title="Template:Crystallization"><abbr title="View this template">v</abbr></a></li><li class="nv-talk"><a href="/wiki/Template_talk:Crystallization" title="Template talk:Crystallization"><abbr title="Discuss this template">t</abbr></a></li><li class="nv-edit"><a href="/wiki/Special:EditPage/Template:Crystallization" title="Special:EditPage/Template:Crystallization"><abbr title="Edit this template">e</abbr></a></li></ul></div></td></tr></tbody></table> <p><br /> In chemistry, <b>fractional crystallization</b> is a stage-wise separation technique that relies on the liquid-solid phase change. fractional crystallisation. This is an old established method which is nevertheless capable of excellent results and a description is available in "The practical Methods of organic Chemistry" by Ludwig Gattermann in 1898 and a translation was available in English by WILLIAM B. SHOBER who was a Lehigh University, USA. </p><p>This technique <a href="/wiki/Fractionation" title="Fractionation">fractionates</a> via differences in crystallization temperature and enables the purification of multi-component mixtures, as long as none of the constituents can act as solvents to the others. Due to the high selectivity of the solid – liquid equilibrium, very high purities can be achieved for the selected component. </p> <meta property="mw:PageProp/toc" /> <div class="mw-heading mw-heading2"><h2 id="Principle_of_separation">Principle of separation</h2><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=1" title="Edit section: Principle of separation"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <p>The crystallization process starts with the partial freezing of the initial <a href="/wiki/Liquid" title="Liquid">liquid</a> mixture by slowly decreasing its temperature. The frozen solid phase subsequently has a different composition than the remaining liquid. This is the fundamental physical principle behind the melt fractionating process and quite comparable to <a href="/wiki/Distillation" title="Distillation">distillation</a>, which operates between a liquid and the gas phase. </p><p>The <a href="/wiki/Crystal" title="Crystal">crystals</a> will grow on a cooled surface or alternatively as a suspension in the liquid. The heat released by the solidification process is withdrawn through a cooling surface or via the liquid. In theory, 100% of the product could be solidified and recovered. In practice, various strategies such as partial melting of the solid fraction (sweating) need to be applied in order to reach high purity levels. </p> <div class="mw-heading mw-heading2"><h2 id="Advantages">Advantages</h2><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=2" title="Edit section: Advantages"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <p>Fractional crystallization has various advantages over other separation technologies. First of all, it makes the purification of close boilers possible. This allows for very high purities even for challenging components. Furthermore, because of the lower operating <a href="/wiki/Temperature" title="Temperature">temperature</a>, the thermal stress applied to the product is very low. This is in particular relevant for products that would otherwise <a href="/wiki/Oligomer" title="Oligomer">oligomerize</a> or <a href="/wiki/Decomposition" title="Decomposition">degrade</a>. Next, fractional crystallization is usually an inherently safe technology, because it operates at low pressures and low temperatures. Also, it does not use any <a href="/wiki/Solvent" title="Solvent">solvents</a> and is emission-free. Finally, since the <a href="/wiki/Latent_heat" title="Latent heat">latent heat</a> of solidification is 3–6x lower than the heat of <a href="/wiki/Evaporation" title="Evaporation">evaporation</a>, the energy consumption is – in comparison to distillation – much lower. </p> <div class="mw-heading mw-heading2"><h2 id="Process_steps">Process steps</h2><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=3" title="Edit section: Process steps"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <p>Fractional crystallization involves several key steps: </p> <ol><li><b>Crystallization</b>: This is the initial phase where the material to be purified is cooled. As it cools, high-purity crystals begin to form on the cooling surface. The purity is achieved because the impurities tend to remain in the liquid phase rather than being incorporated into the crystal structure.</li> <li><b>Draining</b>: After the formation of the crystals, the next step is to remove the residual liquid that contains a higher concentration of impurities. This process of draining helps to separate the pure crystals from the impure liquid.</li> <li><b>Sweating</b>: This phase is a controlled partial melting process. It further purifies the product by melting only a small portion of the crystal. The melting causes the impurities trapped within or between the crystal structures to be released and separated.</li> <li><b>Total Melting</b>: In the final step, the remaining crystallized material, which is now the purified product, is completely melted. This total melting facilitates the removal of the pure substance from the crystallization equipment and prepares it for downstream processing.</li></ol> <div class="mw-heading mw-heading2"><h2 id="Crystallizers">Crystallizers</h2><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=4" title="Edit section: Crystallizers"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <p>There are three differenct fractional crystallization technologies available: </p> <div class="mw-heading mw-heading3"><h3 id="Falling-film">Falling-film</h3><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=5" title="Edit section: Falling-film"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <p>In the falling-film crystallizer, crystals grow from a melt that forms a thin film along the inside of cooled tubes. A concurrent cooling medium flows on the outside of these tubes. This arrangement allows for reproducible and high transfer rates of heat, facilitating the growth of crystals from the falling film of melt. The solid–liquid separation of the resulting slurry can be accomplished using a wash column or a centrifuge. This technology is more complex than others but offers the advantage of high separation efficiency and very high purities. A typical feed has concentrations between 90–99%, which is purified up to 99.99 wt.-% or greater. For example, glacial <a href="/wiki/Acrylic_acid" title="Acrylic acid">acrylic acid</a>, optical grade <a href="/wiki/Bisphenol_A" title="Bisphenol A">bisphenol-A</a> and battery grade <a href="/wiki/Ethylene_carbonate" title="Ethylene carbonate">ethylene carbonate</a> can be purified to their highest grade using a falling-film crystallizer. </p> <div class="mw-heading mw-heading3"><h3 id="Static">Static</h3><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=6" title="Edit section: Static"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <p>The static crystallizer allows crystals to grow from a stagnant melt, making it a versatile and robust technology. It can purify highly challenging products, including those with most challenging properties, such as high viscosities and high or low melting points. Examples of applications include <a href="/w/index.php?title=Isopulegol&action=edit&redlink=1" class="new" title="Isopulegol (page does not exist)">isopulegol</a>, <a href="/wiki/Phosphoric_acid" title="Phosphoric acid">phosphoric acid</a>, <a href="/wiki/Wax" title="Wax">wax</a> and <a href="/wiki/Paraffin_wax" title="Paraffin wax">paraffins</a>, <a href="/wiki/Anthracene" title="Anthracene">anthracene</a> / <a href="/wiki/Carbazole" title="Carbazole">carbazole</a> and even satellite-grade <a href="/wiki/Hydrazine" title="Hydrazine">hydrazine</a>. </p> <div class="mw-heading mw-heading3"><h3 id="Suspension">Suspension</h3><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=7" title="Edit section: Suspension"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <p>In suspension crystallization, crystals are generated on a cooling surface and then scraped off to continue growing in size within a stirred vessel in suspension or slurry. The solid–liquid separation is performed either through a wash-column or a centrifuge. This method is more complex to operate, but offers the advantage of a high separation efficiency, which translates to considerable engery savings. Examples of applications include paraxylene, halogenated aromatics, and also aqueous feeds. </p> <div class="mw-heading mw-heading2"><h2 id="See_also">See also</h2><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=8" title="Edit section: See also"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <ul><li><a href="/wiki/Cold_Water_Extraction" class="mw-redirect" title="Cold Water Extraction">Cold Water Extraction</a></li> <li><a href="/wiki/Fractional_crystallization_(geology)" title="Fractional crystallization (geology)">Fractional crystallization (geology)</a></li> <li><a href="/wiki/Fractional_freezing" title="Fractional freezing">Fractional freezing</a></li> <li><a href="/wiki/Laser-heated_pedestal_growth" title="Laser-heated pedestal growth">Laser-heated pedestal growth</a></li> <li><a href="/wiki/Pumpable_ice_technology" title="Pumpable ice technology">Pumpable ice technology</a></li> <li><a href="/wiki/Recrystallization_(chemistry)" title="Recrystallization (chemistry)">Recrystallization (chemistry)</a></li> <li><a href="/wiki/Seed_crystal" title="Seed crystal">Seed crystal</a></li> <li><a href="/wiki/Single_crystal" title="Single crystal">Single crystal</a></li></ul> <div class="mw-heading mw-heading2"><h2 id="References">References</h2><span class="mw-editsection"><span class="mw-editsection-bracket">[</span><a href="/w/index.php?title=Fractional_crystallization_(chemistry)&action=edit&section=9" title="Edit section: References"><span>edit</span></a><span class="mw-editsection-bracket">]</span></span></div> <ul><li><a rel="nofollow" class="external text" href="https://web.archive.org/web/20160303181456/http://acaschool.iit.edu/lectures04/JLiangXtal.pdf">"Small Molecule Crystalization"</a> (<a href="/wiki/PDF" title="PDF">PDF</a>) at <a href="/wiki/Illinois_Institute_of_Technology" title="Illinois Institute of Technology">Illinois Institute of Technology</a> website</li> <li>"<a rel="nofollow" class="external text" href="https://www.chemengonline.com/facts-at-your-fingertips-fractional-solvent-free-melt-crystallization/">Fractional Solvent-Free Melt Crystallization</a>" at <a rel="nofollow" class="external text" href="https://www.chemengonline.com/">Chemical Engineering</a> website</li> <li><a rel="nofollow" class="external text" href="https://www.sulzer.com/en/products/separation-technology/crystallization">Sulzer Fractional Crystallization Technologies</a></li></ul> <p>C. A. Soch, Fractional Crystallization, The Journal of Physical Chemistry 1898 2 (1), 43-50; DOI: 10.1021/j150001a002 </p> <!-- NewPP limit report Parsed by mw‐web.codfw.main‐f69cdc8f6‐ps8jv Cached time: 20241122150828 Cache expiry: 2592000 Reduced expiry: false Complications: [vary‐revision‐sha1, show‐toc] CPU time usage: 0.181 seconds Real time usage: 0.245 seconds Preprocessor visited node count: 610/1000000 Post‐expand include size: 14461/2097152 bytes Template argument size: 1385/2097152 bytes Highest expansion depth: 13/100 Expensive parser function count: 3/500 Unstrip recursion depth: 0/20 Unstrip post‐expand size: 8986/5000000 bytes Lua time usage: 0.116/10.000 seconds Lua memory usage: 1823181/52428800 bytes Number of Wikibase entities loaded: 0/400 --> <!-- Transclusion expansion time report (%,ms,calls,template) 100.00% 208.439 1 -total 38.15% 79.511 1 Template:Crystallization 36.29% 75.651 1 Template:Infobox 29.68% 61.862 1 Template:Short_description 23.96% 49.939 1 Template:More_footnotes 21.84% 45.517 1 Template:Ambox 17.52% 36.524 2 Template:Pagetype 6.80% 14.169 4 Template:Main_other 6.16% 12.838 1 Template:Use_American_English 5.78% 12.057 1 Template:SDcat --> <!-- Saved in parser cache with key enwiki:pcache:idhash:5782826-0!canonical and timestamp 20241122150828 and revision id 1257981078. 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