# Last edited on 2017-02-07 08:32:07 by jstolfi PROCESSING BEESWAX ---------------------------------------------------------------------- 2017-01-14 Some 105 g of beeswax was bought from the internet (Asher, maybe?). It was dark yellow, barely translucent, with a stain of red ink or dye on one corner. Purifying and clarifying Scraped off the corner and melted the rest in a can over the electric stove. It melted at 62-63 C, as per references, yielding a clear deep orange liquid. Added 5 g of activated carbon to the molten wax. Substantial effervescence; maybe air or other gases trapped in the carbon? Heated to 130 C for some minutes. Filtered at ~100 C through towel paper, into a small rectangular PE box. Surprisingly, the filtrate was totally clear and colorless! Did the carbon adsorb all coloring matters? Perhaps some O2 adsorbed in the carbon helper, by oxidizing them? The residue left on the filter was a hard black waxy solid (clarified beeswax impregnated with carbon powder). ---------------------------------------------------------------------- 2017-01-15 The bleached and filtered beeswax above does not shrink appreciably when freezing, unlike paraffin. Extraction with ethanol Placed some clarified beeswax in ethanol 99% at ~30 C. Does not seem to dissolve visibly. Heated some 2 g of grated beeswax and 15 g of ethanol 99% in a tin can in bainmarie. The wax melted at 60-65 C but still did not dissolve completely in the ethanol. Some of it remained as big oily drops slightly denser than ethanol. Drops were solid at ~55 C. The uberliq was clear, but seems to have deposited additional material on cooling back to 30 C. The solids are white, semicrystalline and hard. 2017-01-20 Attempted to repeat the experiment above in larger quantity, separating the components of beeswax by solubility in ethanol. FIRST EXTRACTION Grated ~16 g of beeswax (clarified as above). Placed in erlen E5 (237 g with flask). Added 81 g of ethanol 99 (Asher). Heated the mix (B0) in bainmarie to 75 C. The wax melted into 2 phases, both clear. On cooling to 70 C, the upper phase of (B0) remained clear but the lower one became translucent. The bottom layer seemed to grow an outer transparent layer as it cooled to 65 C. The uberliq remained clear as it cooled to 60 C, but then became cloudy. Reheated at 75 C. Separated again in 2 clear phases, but now the bottom one was slightly cloudy. At 72 C the bottom phase was still liquid but milky. Decanted the top phase (B1) of (B0) at 70 C into erlen E1 (85 g; 309 g with flask), leaving the bottom one (B2) in erlen E5. Heated (B2) to 80 C to drive off any remaining ethanol. (But some may have remained dissolved. Seems hard to drive off entirely, even on heating at 90 C as in following runs.) Result was a clear oily liquid (B3). Poured (B3) into beaker B7 and weighted: ~13 g. Cooling the ethanolic extract (B1) to 10 C in an ice bath resulted in a fluffy white ppt floating in liquid. Filtered (B1) at 10 C with Qualy paper 150 mm. Filtrate (B4) of (B1) dropped into erlen E5; total 300 g with flask. The ppt (B5) of (B1) was a white waxy powder: wet weight 5g, dry weight ~1 g. The powder did not show any tendency to clump while drying. SECOND EXTRACTION Suspected that not all the ethanol-soluble fraction had been extracted, because (B1) may have been saturated with it. To check that, the extraction was repeated a second time. The insoluble phase (B3) and the filtrate (B4) were placed again in erlen E5 as (B0a) and heated again in bainmarie to ~78 C (when ethanol barely started boiling). On cooling to 70 C the upper phase of (B0a) was a bit cloudy this time, but clarified on standing a few minutes. Decanted again the upper phase (B6) of (B0a) into erlen E1. About 73 g (285 g with flask) of clear colorless liquid. The lower phase (B7), a clear oily liquid, was heated to ~90 C to drive out the remaining ethanol, then poured in a beaker. It became ~13 g of a hard white solid. On cooling (B6) a white fluffy ppt formed at ~50 C, and more came out as it was cooled to ~10 C. Filtered (B6) at 10 C, on Qualy paper; washing with 3 g of ethanol 99%. The ppt (B8) was a white waxy powder, ~4 g wet, < 1 g dry. The filtrate (B9) of (B6) was about 73 g of clear colorless liquid. THIRD EXTRACTION Combined the filtrate (B9) of (B6) and the lower phase (B7) of (B0a) into erlen E5, as (B0b). Heated (B0b) n bainmarie as before to ~78 C (when ethanol was almost boiling). Decanted at 70 C into the upper phase (B11) and the lower oily phase (B2), both clear. Heated the oily phase (B12) at 85 C to remove the remaining ethanol, and poured into beaker B7. On cooling became 12 g of hard white solid. Reheated the filtrate (B11) to 70 C, then cooled to 12 C. Yielded a white fluffy ppt. Filtered at ~12 C (spilled about 2 ml by accident). The filtrate (B13) of (B11) was 63 g of clear liquid. (Lost 4-5 g in filter paper.) Diluting a bit of (B13) with water resulted in a slightly milky liquid, but no immediate ppt. That indicates that (B13) still contains some dissolved wax component, but very little. The ppt (B14) of (B11) was again a white powder; the dry weight was < 1 g. Visually, the amount seemed to be less than what was obtained in the previous extractions. FOURTH EXTRACTION For this last extraction pass, decided to use fresh ethanol instead of reusing the (B13) filtrate. Placed the solid waxy component (B12) (12 g) into erlen E5 with 50 g of fresh ethanol 99%. Heated the mix (B0c) to 70 C in bainmarie and decanted the two liquid phases as before. The lower oily phase (B16) was heated to 85 C to remove the remaining ethanol, then poured into a beaker. On cooling it became 11 g of a hard white solid, that started solidifying at ~57 C. The upper phase (B15) of (B0c) was cooled to 10 C. It started to form a white fluffy ppt at ~45 C. It was filtered at 10 C The clear filtrate (B17) of (B15) was merged with the filtrate (B13) of the third extraction, yielding 125 ml of clear liquid. The ppt (B18) of (B15) was again a white powder, simlar to (B5), (B8), and (B14), but in much smaller amount. All precipitates (B5), (B8), (B14), and (B18) were merged and saved. Total weight ~2 g. CONCLUSION It seems that 16 g of beeswax contains ~2 g of some components that can be extracted by anhydrous ethanol at 70-78 C, but precipitate out almost completely when cooling to 10 C. About 150 g of ethanol are required to dissolve those components. The residue from such extraction is a hard waxy solid that starts to melt at ~56 C. ---------------------------------------------------------------------- 2017-02-05 Sat The ethanol (B13)+(B17) had deposited a thin waxy film at the bottom, nearly transparent. The film was loose and floated about in the ethanol. Filtered (B13)+(B17) with W201 paper into a 250 ml amber bottle. Discarded the waxy films.