Sulfur in extracts

Hey there! Would you care to elaborate on how I’d incorporate inline? Such as volume of copper to volume of material being extracted etc, I ran into this issue a bunch last year and wish I would have learned this earlier. Thanks in advance for any input :metal:t2:

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My apologies, I found the other post and will dig deeper .

I don’t have any quantifying data for removal of sulfur. I noted that used copper for several runs left a rotten egg smell on the spent copper

I’m currently dealing with a large amount of sulfur treated material. We’ve tried everything we can think of with copper;
Copper scrubbies and then powder in-line were helping but didn’t get it all out.
Copper powder directly in the solution for 48 hours seemed to help a lot more. still waiting on tests to come back
(BHO)

What seems to work is distillation. The fart smell comes out with the volatiles, most likely from the residual solvent. Fart smell loves to stick in your ethanol. The boiling point of sulfur is like 800f, so I’m guessing it stays in the boiling flask… regardless, the disty comes out clean.

We still have probly couple thousand pounds to go through so if anyone knows a really easy trick that really works for BHO, I’d love to hear. Maybe more powder inline? Anyone have a ratio that’s worked for them?

Ty

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Interested in this as well.

Spitballing here…

setup a recirculating style CRC and fill it with copper scrubbies or even the powdered copper rather than the traditional magic dirts. see: Opaline Silica Thread for 1k word substitute.

@Photon_noir used a foodboxer.
@Soxhlet is using a gear pump.
@Roguelab points out that most recovery pumps can handle liquid too.

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Pack a column with these maybe? Threaded and gasketed stainless filter housing, run two with a three way valve to allow you to line up to either as well as a bypass. Run length of column and flow rate testing to determine optimal size and flow rate as well as time to fouling. you could also stack the coils of mesh on a central rod with stop plates above and below (rated for your solvent of choice) creating a diy filter cartridge. That would speed up replacement time when you need to swap media.

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@cyclopath Brilliant! This is a good plan.

@Estokha Now we’re cookin! I’ve seen the DIY “sintered disc” using this method.

The more copper the merrier!

I’m gonna try a hexane soak in powdered copper today. If it works I will built something proper.

Thanks, team!

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Sorry I missed this for over a month.

THAT is the stuff, @Estokha!

@cyclopath That stuff also makes a damn fine Faraday cage when you line the walls and ground it… you know, just fyi. :smile:

Actually, @midsfactory, you have met the problem well with various solutions. However, while powder can be faster (IF it is very clean and free of oxide), it can really only be used once with any simplicity. Cleaning oxides off of tiny copper dust particles can be an exercise in futility, since they might just be almost entirely composed of oxide, being so small! The same goes for the copper*sulfur reaction product… it may comprise the entire particle by the time it’s done reacting… so you cannot clean it up with citric acid and reuse it, the way you can reuse copper scrubby mesh. A likely more pernicious problem with copper dust is reacting it with anything can simply cause it to dissolve!

To speed up the reaction of sulfur compounds with metallic copper, heat and moisture help.

Why not just use an adsorbent for that pesky elemental sulfur you think remains after the copper?

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@Photon_noir great timing actually! I had put this project on the back burner until yesterday.

This is what I’ve done:
I performed a cold ethanol extraction followed by a quick particulate filter through a Buchner. I took my solution and split it between two 5000ml flasks. I added 50g copper “chops” to each. I put one flask in a hot plate and left one room temp. I didn’t start to see a reaction until about 130f. The room temp flask never reacted.
I kept adding more copper chop until the reaction stopped. Then I had to go home. Today I’m going to filter out the copper chops (diatomaceous earth + Buchner?), roto and send in some tests. Also going to distill the crude to see if I get any more crazy isomers.

My questions are:
Testing for sulfur? Any way to do at my lab without analytical instruments?
Sulfur in my solvent? Would it linger?
Cleaning copper chops? Citric acid wash? @Photon_noir gave many warnings on the difficulty of cleaning the copper.

Could there by a better way to perform the reaction in general? I’m most likely going to do this in 5 gal buckets to scale up…

Thanks!!

Thanks again!!

What about liquid-liquid removal of the sulfur in an aqueous solution followed by a pass through a molecular sieve?

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Thatis obviously the best way, it’s just a lot more equipment/processing we are willing to put into this. It’s about 10000lb. 3000 of it is leaf and trim…

A neighbor of mine is having success with copper, but they are being tight lipped. (Probably reading this too)

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@midsfactory Not sure if this test for sulfur will be sensitive enough? But sharing anyway :man_shrugging:

https://www.canada.ca/en/conservation-institute/services/conservation-preservation-publications/canadian-conservation-institute-notes/test-sulfur-acetate-paper.html

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https://patents.google.com/patent/US6743405

https://patents.google.com/patent/EP1633475A1

Both of these are interesting, the second uses a Zeolite to remove sulfur from liquid or gas streams.

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Looks like it could work, mainly for my solvent. There is actually naturally a curing sulfur in plants, so it might not help testing crude. Worth a go though!

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Wooo! My little brain needs some coffee for focus on these :slight_smile: ty friend

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13x beads and copper in conjunction? Lle seems to be best methanol water and hexane? @midsfactory

Depends on solubility but works well to remove some pests @midsfactory

I’m hoping to skip LLE and just try adsorbents. The material isn’t worth the added cost of LLE.

Youll have great success if you use a copper salt that will pull sulfur into water layer .

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