{"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 class=\"wp-block-paragraph\"><strong>Still with 60&#8243; packed Reflux column in operation<\/strong><\/p>\n\n\n\n<p class=\"wp-block-paragraph\">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=\"JqMR98SuEG\"><a href=\"https:\/\/graywolf.moveweight.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; visibility: hidden;\" title=\"\u201c10.19 190 Proof Ethanol from scratch\u201d \u2014 GrayWolf&amp;apos;s Lair\" src=\"https:\/\/graywolf.moveweight.com\/index.php\/10-the-alchemist-resource\/10-19-190-proof-ethanol-from-scratch\/embed\/#?secret=plhN7qULN4#?secret=JqMR98SuEG\" data-secret=\"JqMR98SuEG\" 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=\"gNlXkRps9z\"><a href=\"https:\/\/graywolf.moveweight.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; visibility: hidden;\" title=\"\u201c15.8 Ethanol fractionating still\u201d \u2014 GrayWolf&amp;apos;s Lair\" src=\"https:\/\/graywolf.moveweight.com\/index.php\/15-diy-equipment\/15-8-ethanol-fractionating-still\/embed\/#?secret=5OSnMFhN1I#?secret=gNlXkRps9z\" data-secret=\"gNlXkRps9z\" width=\"525\" height=\"296\" frameborder=\"0\" marginwidth=\"0\" marginheight=\"0\" scrolling=\"no\"><\/iframe>\n<\/div><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\">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 loading=\"lazy\" decoding=\"async\" width=\"767\" height=\"1024\" src=\"https:\/\/graywolf.moveweight.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-767x1024.webp\" alt=\"\" class=\"wp-image-1725\" srcset=\"https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-767x1024.webp 767w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-225x300.webp 225w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-768x1026.webp 768w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-1150x1536.webp 1150w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-600x801.webp 600w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Vacuum-still-jpg.webp 1500w\" sizes=\"auto, (max-width: 767px) 100vw, 767px\" \/><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\"><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 loading=\"lazy\" decoding=\"async\" width=\"1024\" height=\"988\" src=\"https:\/\/graywolf.moveweight.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-1024x988.webp\" alt=\"\" class=\"wp-image-1726\" srcset=\"https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-1024x988.webp 1024w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-300x289.webp 300w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-768x741.webp 768w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-600x579.webp 600w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Reflux-colum-stuffing-jpg.webp 1500w\" sizes=\"auto, (max-width: 1024px) 100vw, 1024px\" \/><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\"><strong>Pot scrubber column stuffing from Hong\u2019s Restaurant Suply<\/strong><\/p>\n\n\n\n<p class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 loading=\"lazy\" decoding=\"async\" width=\"1024\" height=\"871\" src=\"https:\/\/graywolf.moveweight.com\/wp-content\/uploads\/2023\/04\/column-head-1024x871.webp\" alt=\"\" class=\"wp-image-1728\" srcset=\"https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-1024x871.webp 1024w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-300x255.webp 300w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-768x653.webp 768w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-600x510.webp 600w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/column-head-jpg.webp 1500w\" sizes=\"auto, (max-width: 1024px) 100vw, 1024px\" \/><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\"><strong>Column head with thermocouple and compound pressure gauge<\/strong><\/p>\n\n\n\n<p class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 loading=\"lazy\" decoding=\"async\" width=\"1024\" height=\"694\" src=\"https:\/\/graywolf.moveweight.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-1024x694.webp\" alt=\"\" class=\"wp-image-1729\" srcset=\"https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-1024x694.webp 1024w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-300x203.webp 300w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-768x520.webp 768w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-600x406.webp 600w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Air-heat-exchanger-jpg.webp 1500w\" sizes=\"auto, (max-width: 1024px) 100vw, 1024px\" \/><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\"><strong>3\/8\u201d 10 pass single row copper vapor to air heat exchanger using Derale components<\/strong><\/p>\n\n\n\n<p class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 loading=\"lazy\" decoding=\"async\" width=\"779\" height=\"1024\" src=\"https:\/\/graywolf.moveweight.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-779x1024.webp\" alt=\"\" class=\"wp-image-1732\" srcset=\"https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-779x1024.webp 779w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-228x300.webp 228w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-768x1010.webp 768w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-1168x1536.webp 1168w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-600x789.webp 600w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Collection-jar-2-jpg.webp 1500w\" sizes=\"auto, (max-width: 779px) 100vw, 779px\" \/><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\"><strong>Thumper lid attachment from Nor Cal Brewing Solutions<\/strong><\/p>\n\n\n\n<p class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\"><strong>Oops, New Reflux Still Column Sizing Insights!<\/strong><\/p>\n\n\n\n<p class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 class=\"wp-block-paragraph\">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 loading=\"lazy\" decoding=\"async\" width=\"1024\" height=\"902\" src=\"https:\/\/graywolf.moveweight.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-1024x902.webp\" alt=\"\" class=\"wp-image-1734\" srcset=\"https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-1024x902.webp 1024w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-300x264.webp 300w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-768x677.webp 768w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-600x529.webp 600w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-pot-in-beads-jpg.webp 1500w\" sizes=\"auto, (max-width: 1024px) 100vw, 1024px\" \/><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\"><strong>Large Pot in Bead Bath<\/strong><\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><img loading=\"lazy\" decoding=\"async\" width=\"532\" height=\"1024\" src=\"https:\/\/graywolf.moveweight.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-532x1024.webp\" alt=\"\" class=\"wp-image-1735\" srcset=\"https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-532x1024.webp 532w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-156x300.webp 156w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-768x1479.webp 768w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-798x1536.webp 798w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-1064x2048.webp 1064w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-600x1155.webp 600w, https:\/\/graywolfslair.com\/wp-content\/uploads\/2023\/04\/Large-reflux-still-1-scaled.webp 1330w\" sizes=\"auto, (max-width: 532px) 100vw, 532px\" \/><\/figure>\n\n\n\n<p class=\"wp-block-paragraph\"><strong>Large Pot In Operation Insulated and Wrapped<\/strong><\/p>\n\n\n\n<p class=\"wp-block-paragraph\">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":{"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 v28.1 - https:\/\/yoast.com\/product\/yoast-seo-wordpress\/ -->\n<title>15.8.1 Refluxing columns for producing 190 proof Ethanol - GrayWolf&#039;s Lair<\/title>\n<meta name=\"robots\" content=\"index, follow, max-snippet:-1, max-image-preview:large, max-video-preview:-1\" \/>\n<link rel=\"canonical\" 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