{"id":535,"date":"2023-01-10T23:46:32","date_gmt":"2023-01-10T23:46:32","guid":{"rendered":"https:\/\/graywolfslair.com\/?p=535"},"modified":"2023-04-05T20:55:25","modified_gmt":"2023-04-05T20:55:25","slug":"15-8-1-refluxing-columns-for-producing-190-proof-ethanol","status":"publish","type":"post","link":"https:\/\/graywolfslair.com\/index.php\/15-diy-equipment\/15-8-ethanol-fractionating-still\/15-8-1-refluxing-columns-for-producing-190-proof-ethanol\/","title":{"rendered":"15.8.1 Refluxing columns for producing 190 proof Ethanol"},"content":{"rendered":"\n<p><strong>Still with 60&#8243; packed Reflux column in operation<\/strong><\/p>\n\n\n\n<p>In previous articles 10.19 190 Proof Ethanol from Scratch, and article 15.8 Ethanol Fractionating Still, I discus how to produce 190 proof Ethanol, the difference being that the latter uses a reflux column to achieve 95% 190 proof concentration, while the former uses multiple runs in a vacuum pot still and mol sieve desiccant to achieve that end.<\/p>\n\n\n\n<figure class=\"wp-block-embed is-type-wp-embed is-provider-graywolf-039-s-lair wp-block-embed-graywolf-039-s-lair\"><div class=\"wp-block-embed__wrapper\">\n<blockquote class=\"wp-embedded-content\" data-secret=\"q4xMyVsbWC\"><a href=\"https:\/\/graywolfslair.com\/index.php\/10-the-alchemist-resource\/10-19-190-proof-ethanol-from-scratch\/\">10.19 190 Proof Ethanol from scratch<\/a><\/blockquote><iframe loading=\"lazy\" class=\"wp-embedded-content\" sandbox=\"allow-scripts\" security=\"restricted\" style=\"position: absolute; clip: rect(1px, 1px, 1px, 1px);\" title=\"&#8220;10.19 190 Proof Ethanol from scratch&#8221; &#8212; GrayWolf&#039;s Lair\" src=\"https:\/\/graywolfslair.com\/index.php\/10-the-alchemist-resource\/10-19-190-proof-ethanol-from-scratch\/embed\/#?secret=H18n0H1osK#?secret=q4xMyVsbWC\" data-secret=\"q4xMyVsbWC\" width=\"525\" height=\"296\" frameborder=\"0\" marginwidth=\"0\" marginheight=\"0\" scrolling=\"no\"><\/iframe>\n<\/div><\/figure>\n\n\n\n<figure class=\"wp-block-embed is-type-wp-embed is-provider-graywolf-039-s-lair wp-block-embed-graywolf-039-s-lair\"><div class=\"wp-block-embed__wrapper\">\n<blockquote class=\"wp-embedded-content\" data-secret=\"Eq2AwfzKnJ\"><a href=\"https:\/\/graywolfslair.com\/index.php\/15-diy-equipment\/15-8-ethanol-fractionating-still\/\">15.8 Ethanol fractionating still<\/a><\/blockquote><iframe loading=\"lazy\" class=\"wp-embedded-content\" sandbox=\"allow-scripts\" security=\"restricted\" style=\"position: absolute; clip: rect(1px, 1px, 1px, 1px);\" title=\"&#8220;15.8 Ethanol fractionating still&#8221; &#8212; GrayWolf&#039;s Lair\" src=\"https:\/\/graywolfslair.com\/index.php\/15-diy-equipment\/15-8-ethanol-fractionating-still\/embed\/#?secret=rcpSyHufHm#?secret=Eq2AwfzKnJ\" data-secret=\"Eq2AwfzKnJ\" width=\"525\" height=\"296\" frameborder=\"0\" marginwidth=\"0\" marginheight=\"0\" scrolling=\"no\"><\/iframe>\n<\/div><\/figure>\n\n\n\n<p>Underneath the towels, my test still is composed of a 6\u201d X 12\u201d boiling pot, with 5\u2019 of 2\u201d sanitary tubing stuffed with stainless steel ribbon from commercial pot scrubbers.<\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img data-recalc-dims=\"1\" loading=\"lazy\" decoding=\"async\" width=\"525\" height=\"701\" src=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-767x1024.webp?resize=525%2C701&#038;ssl=1\" alt=\"\" class=\"wp-image-1725\" srcset=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp?resize=767%2C1024&amp;ssl=1 767w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp?resize=225%2C300&amp;ssl=1 225w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp?resize=768%2C1026&amp;ssl=1 768w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp?resize=1150%2C1536&amp;ssl=1 1150w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp?resize=600%2C801&amp;ssl=1 600w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp?w=1500&amp;ssl=1 1500w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp?w=1050 1050w\" sizes=\"auto, (max-width: 525px) 100vw, 525px\" \/><\/figure>\n\n\n\n<p><strong>Vacuum still assembly with 36\u201d column showing bead bath heating<\/strong><\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img data-recalc-dims=\"1\" loading=\"lazy\" decoding=\"async\" width=\"525\" height=\"507\" src=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-1024x988.webp?resize=525%2C507&#038;ssl=1\" alt=\"\" class=\"wp-image-1726\" srcset=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-jpg.webp?resize=1024%2C988&amp;ssl=1 1024w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-jpg.webp?resize=300%2C289&amp;ssl=1 300w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-jpg.webp?resize=768%2C741&amp;ssl=1 768w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-jpg.webp?resize=600%2C579&amp;ssl=1 600w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-jpg.webp?w=1500&amp;ssl=1 1500w\" sizes=\"auto, (max-width: 525px) 100vw, 525px\" \/><\/figure>\n\n\n\n<p><strong>Pot scrubber column stuffing from Hong\u2019s Restaurant Suply<\/strong><\/p>\n\n\n\n<p>The boiling pot sits in a commercial electric soup pot full of aluminum beads supplied by Cascade Sciences, and there is a thermocouple in the boiling pot attached to a PID for heat control, and a thermocouple in the column head to determine the boiling point of the fraction currently in the column head.<\/p>\n\n\n\n<p>The thermocouples were custom 1\/8\u201d Type J made by Wilcon Industries and inserted through 1\/8\u201d Swagelok compression fittings, that I through drilled so the thermocouple could pass all the way through.<\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img data-recalc-dims=\"1\" loading=\"lazy\" decoding=\"async\" width=\"525\" height=\"447\" src=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-1024x871.webp?resize=525%2C447&#038;ssl=1\" alt=\"\" class=\"wp-image-1728\" srcset=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-jpg.webp?resize=1024%2C871&amp;ssl=1 1024w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-jpg.webp?resize=300%2C255&amp;ssl=1 300w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-jpg.webp?resize=768%2C653&amp;ssl=1 768w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-jpg.webp?resize=600%2C510&amp;ssl=1 600w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-jpg.webp?w=1500&amp;ssl=1 1500w\" sizes=\"auto, (max-width: 525px) 100vw, 525px\" \/><\/figure>\n\n\n\n<p><strong>Column head with thermocouple and compound pressure gauge<\/strong><\/p>\n\n\n\n<p>I insulated the column with 1\u201d thick closed cell foam 2 1\/8\u201d pipe insulation and all hoses are 3\/8\u201d 304 stainless steel over braided PTFE with #6 JIC connectors.<\/p>\n\n\n\n<p>For a condenser I used a 10 pass single row copper tube heat exchanger with aluminum fins and added a blower from another double row heat exchanger.<\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img data-recalc-dims=\"1\" loading=\"lazy\" decoding=\"async\" width=\"525\" height=\"356\" src=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-1024x694.webp?resize=525%2C356&#038;ssl=1\" alt=\"\" class=\"wp-image-1729\" srcset=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-jpg.webp?resize=1024%2C694&amp;ssl=1 1024w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-jpg.webp?resize=300%2C203&amp;ssl=1 300w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-jpg.webp?resize=768%2C520&amp;ssl=1 768w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-jpg.webp?resize=600%2C406&amp;ssl=1 600w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-jpg.webp?w=1500&amp;ssl=1 1500w\" sizes=\"auto, (max-width: 525px) 100vw, 525px\" \/><\/figure>\n\n\n\n<p><strong>3\/8\u201d 10 pass single row copper vapor to air heat exchanger using Derale components<\/strong><\/p>\n\n\n\n<p>For a collection jar, I used a thumper lid from Nor Cal Brewing Solutions.&nbsp; It is set up with a connection to the test sled vacuum pump, so the system can also be run under -23\u201d Hg vacuum as a vacuum still.<\/p>\n\n\n\n<p>I will be running vacuum still experiment for comparison once I establish a baseline.<\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img data-recalc-dims=\"1\" loading=\"lazy\" decoding=\"async\" width=\"525\" height=\"690\" src=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-779x1024.webp?resize=525%2C690&#038;ssl=1\" alt=\"\" class=\"wp-image-1732\" srcset=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp?resize=779%2C1024&amp;ssl=1 779w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp?resize=228%2C300&amp;ssl=1 228w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp?resize=768%2C1010&amp;ssl=1 768w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp?resize=1168%2C1536&amp;ssl=1 1168w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp?resize=600%2C789&amp;ssl=1 600w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp?w=1500&amp;ssl=1 1500w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp?w=1050 1050w\" sizes=\"auto, (max-width: 525px) 100vw, 525px\" \/><\/figure>\n\n\n\n<p><strong>Thumper lid attachment from Nor Cal Brewing Solutions<\/strong><\/p>\n\n\n\n<p>For my first run, I diluted 190 proof Ethanol 50\/50 with water, to produce about a 95 proof and put it through the still with a 2\u201d X 36\u201d reflux column in one pass.&nbsp; After it cooled down, the 36\u201d column produced 185 proof ethanol, so I added another 24\u201d of packed reflux column to see what that would produce.&nbsp;<\/p>\n\n\n\n<p>At 26C\/78.8F a single pass measured 195 proof, which when adjusted for temperature above 16C\/60F comes out 190 proof.<\/p>\n\n\n\n<p><strong>Oops, New Reflux Still Column Sizing Insights!<\/strong><\/p>\n\n\n\n<p>Sooooo, I was so elated with achieving my 190 proof azeotropic balance goal with my small still, that I failed to consider all the variables using a larger boiling pot.&nbsp;<\/p>\n\n\n\n<p>Sometimes experiments verify and support pet hypothesis, and sometimes they fly in the face of them for obvious reasons, which I failed to adequately consider.<\/p>\n\n\n\n<p>In this case I attached the same 2\u201d X 60\u201d packed reflux column to the 12\u201d X 12\u201d pot, vis a vis the 6\u201d X 6\u201d still base and expected similar results, despite the 4X difference in surface boiling area producing vapors.<\/p>\n\n\n\n<p>As a result, I only achieved 180 proof in a single pass, demonstrating that I need more refluxing mass cooling down the vapors, so that only the lowest boiling point reach the column head.<\/p>\n\n\n\n<p>I again packed my boiling pot in aluminum beads from Cascade Sciences for even heating, but this time used a 14\u201d baking pan sitting on a Chemorec 2 hot plate, instead of an electric soup pot.<\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img data-recalc-dims=\"1\" loading=\"lazy\" decoding=\"async\" width=\"525\" height=\"462\" src=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-1024x902.webp?resize=525%2C462&#038;ssl=1\" alt=\"\" class=\"wp-image-1734\" srcset=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-jpg.webp?resize=1024%2C902&amp;ssl=1 1024w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-jpg.webp?resize=300%2C264&amp;ssl=1 300w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-jpg.webp?resize=768%2C677&amp;ssl=1 768w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-jpg.webp?resize=600%2C529&amp;ssl=1 600w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-jpg.webp?w=1500&amp;ssl=1 1500w\" sizes=\"auto, (max-width: 525px) 100vw, 525px\" \/><\/figure>\n\n\n\n<p><strong>Large Pot in Bead Bath<\/strong><\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img data-recalc-dims=\"1\" loading=\"lazy\" decoding=\"async\" width=\"525\" height=\"1011\" src=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-532x1024.webp?resize=525%2C1011&#038;ssl=1\" alt=\"\" class=\"wp-image-1735\" srcset=\"https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp?resize=532%2C1024&amp;ssl=1 532w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp?resize=156%2C300&amp;ssl=1 156w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp?resize=768%2C1479&amp;ssl=1 768w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp?resize=798%2C1536&amp;ssl=1 798w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp?resize=1064%2C2048&amp;ssl=1 1064w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp?resize=600%2C1155&amp;ssl=1 600w, https:\/\/i0.wp.com\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp?w=1330&amp;ssl=1 1330w\" sizes=\"auto, (max-width: 525px) 100vw, 525px\" \/><\/figure>\n\n\n\n<p><strong>Large Pot In Operation Insulated and Wrapped<\/strong><\/p>\n\n\n\n<p>The run was smooth and uneventful, but demonstrated the need for more reflux area, which I don\u2019t have room for in my kitchen, so will have to wait until I can move back in my garage lab\/workshop or go to a larger diameter column.<\/p>\n","protected":false},"excerpt":{"rendered":"<p>Still with 60&#8243; packed Reflux column in operation In previous articles 10.19 190 Proof Ethanol from Scratch, and article 15.8 Ethanol Fractionating Still, I discus [&hellip;]<\/p>\n","protected":false},"author":4,"featured_media":0,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_jetpack_memberships_contains_paid_content":false,"footnotes":""},"categories":[79],"tags":[],"class_list":["post-535","post","type-post","status-publish","format-standard","hentry","category-15-8-ethanol-fractionating-still"],"yoast_head":"<!-- This site is optimized with the Yoast SEO plugin v27.4 - https:\/\/yoast.com\/product\/yoast-seo-wordpress\/ -->\n<title>15.8.1 Refluxing columns 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