careysub
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SS Bottle for High Temp Rxn Vessel?
I had the idea of adapting one of these $33 304 (18/8) stainless steel bottles for a 800 mL high temp reaction flask (higher than borosilicate can
tolerate):
http://www.rei.com/product/838945/klean-kanteen-polished-sta...
To make a delivery tube I was thinking using stainless steel tubing brazed to a hole drilled in the lid (or the bottle near the top).
Nearly all stainless steel bottles on the market have plastic caps, sometimes they hide crucial plastic parts (like the threading) inside a "metal
cap", so it can be hard to determine whether it can be used in an all-metal configuration.
An example of this is this $18 one, with I initially liked:
http://www.ecovessel.com/bold-stainless-steel-water-bottle-w...
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Praxichys
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"Cap is made from a single piece of stainless steel and finished with attractive bamboo wood and a small silicone gasket; handwash
the wood cap and dry immediately"
I can imagine that all water bottles have a gasket of some sort. Sealing at the top might be your biggest issue. How hot do you need to get it?
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careysub
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The decorative bamboo inlay and the silicone gasket would have to go. You might come up with your own high temperature replacement gasket material if
necessary - probably a kiln-type ceramic fiber gasket.
Replacing a gasket is not a big deal, it is much easier than trying to replace a threaded plastic piece that makes the first-order seal in other
bottles.
The vessel would be operated exclusively in the vertical position (not tipped higgledy-piggledy as when used as a water bottle), and would rely
primarily on the metal-to-metal threading for the seal. It would operated at atmospheric pressure, like usual chemistry reactions.
If necessary you could bleed inert gas into the vessel though another tube to keep out air.
I was targeting the temperature range above 300C (the continuous service limit of boro), perhaps up to 700 C or so. Brazing alloys are good at least
up to that temp. You could probably push it higher.
I was thinking of brazing rather than welding since it can be done with an oxy-MAPP torch, and I have no welding experience or equipment.
An example of a reaction I was thinking of running with this is the Tarbutton phosphoryl chloride synthesis:
http://www.sciencemadness.org/talk/viewthread.php?tid=13136
which is run in the temperature range of 350-600C.
[Edited on 6-11-2014 by careysub]
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careysub
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Another thought I just had was to use the type of stainless steel bottle that has a plastic plug-type cap, and use the plastic plug to make a mold,
and fill the mold with a high temperature ceramic material. Thermal expansion issues would then need to be taken into account.
The plastic plug steel bottles are available at one third to one quarter the cost of the one I cited:
http://www.ebay.com/itm/Cycling-Bike-Bicycle-Stainless-Steel...
I took a look at the thermal expansion problem. SS 304 has a COTE of 17.6 per million per K, alumina has a COTE of about 7.6, for a difference of one
part per 100,000 per K. It the temperature change is 600 K, then the difference is 6 parts per thousand. if the plug is 50 mm across, this translates
into a total gap of 0.3 mm opening up (0.15 mm per side).
Perhaps using an SS sheet gasket would do the trick.
Here is a nifty paper about how to slip cast refractories:
http://nvlpubs.nist.gov/nistpubs/jres/23/jresv23n2p319_A1b.p...
(file size was too big to upload).
[Edited on 6-11-2014 by careysub]
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careysub
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And another thought - perhaps a plug could be made through "thermite casting"?
Has anyone tried (and succeeded) at casting metal parts using a thermite reaction?
Plain conventional thermite might work, producing an iron plug, though COTE is a bit lower than SS 304. Iron-chromium thermite for an alloy?
Copper COTE is almost identical to SS 304, perhaps Cu2O thermite, with the addition of flux or copper metal to cool/slow the reaction down even more?
Phosphoryl chloride and copper don't play well together I think, so not a good idea for that particular reaction.
[Edited on 6-11-2014 by careysub]
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j_sum1
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Might you also create a metal-metal seal by sharpening the edge and using a soft metal for a gasket? I am thinking copper. The gasket would be a
single use and soft enough to deform when screwed tight. I know that Indium has been used for this purpose traditionally but the MP is way too low.
(This method was the one employed at a place I once worked with water-jet cutting at 55000psi.)
Alternatively, you might wind some thin foil around the thread in a manner similar to teflon tape. When you tighten you create the metal-metal seal.
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Morgan
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If you didn't want to deal with wide mouth bottles something like this is kind of different. At thrift stores/bargain stores I see stainless steel
water bottles, often new for only 2 dollars. But the ones with the metal caps more rare. You would have to make your own cap or could possibly swage
the neck around something if you had the tools with these beer bottles. Rereading the post, these might not have enough volume if you needed
something larger.
http://deepwoodbrew.com/stainless-steel-bottles/9-stainless-...
I have one of these with the very heavy solid steel cap but you would still need a high temperature gasket. One time I bought some gasket material
from an auto store. I don't know how hot it could get but probably pretty good. It was a gray fibrous material you could cut with scissors.
http://www.homebrewing.org/product.asp?itemid=4264&utm_s...
I also have one like this narrow bottle on the left if you scroll down. It has a thick steel screw lid as well with fine threads and O ring or some
kind rubber material, silicone or something.
http://www.bottless.net/Stainless_Steel_Growlers_s/553.htm
Often the cheaper stainless steel water bottles have a press-fit aluminum fine threaded ring in the neck sometimes anodized a different color which I
don't like. It's the same as in the aluminum bottles, it looks like steel but isn't.
[Edited on 7-11-2014 by Morgan]
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careysub
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Thanks for pointing these out! These are very nifty.
There is a role for different sizes of reaction vessel, a cheap 360 mL SS bottle has plenty of uses, besides I usually like to start small with a new
process.
What is especially nice about the SS beer bottle is that you can use a hand capper and put a cap on the bottle after loading your reaction mix. A hole
just right for the receiving tube (or pressure release if the reactants stay in the bottle) can then be made in the cap. I doubt special sealing will
even be necessary. After the reaction is done you just pop the cap off to empty and clean.
These also might be good for storing reagents long-term.
| Quote: | | I have one of these with the very heavy solid steel cap but you would still need a high temperature gasket. One time I bought some gasket material
from an auto store. I don't know how hot it could get but probably pretty good. It was a gray fibrous material you could cut with scissors.
|
I am looking at this ceramic paper as a gasket material:
http://www.seattlepotterysupply.com/Merchant2/merchant.mvc?S...
Although it is not in the same high temperature league, replacing the 1" O-ring in one of the 1 L or 2 L bottles with a PTFE ring could be useful, for
example an alkali fusion reaction that would attack glass:
http://www.mcmaster.com/#o-rings/=uhsbo9
PTFE is of course famously inert, and its ultimate service temperature (one-time use) is its melting point at 335 C.
Yes these are good for a large reaction vessel, and the cap is nice. The threading looks solid enough the the gasket may be unnecessary, or could be
replaced by a refractory clay caulk applied for the run.
[Edited on 7-11-2014 by careysub]
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Morgan
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I bought a couple of these bottles today at a store called TJ MAXX. They are an 18/10 INOX stainless steel. The ones I bought are for dispensing olive
oil with a spout and ribbed silicone stopper. What I like about them is how light they are with a mirror polish.
http://www.cookishop.com/olipac/11763-burette-inox-coffret-e...
http://www.olipac.it/gallery.html
http://www.cultivarplus.it/prodotto.htm
http://www.cultivarplus.it/bottiglia.htm
[Edited on 19-2-2015 by Morgan]
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Magpie
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Sheet graphite is also to be considered for gaskets.
The single most important condition for a successful synthesis is good mixing - Nicodem
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Zombie
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How about a small engine exhaust gasket or a compression washer as found on a spark plug?
The small engine deals are usually 15 - 30mm in diameter, and found on FleaBay for 3-4 bucks.
They tried to have me "put to sleep" so I came back to return the favor.
Zom.
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Molecular Manipulations
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I use copper for high temperature and low/high pressure gaskets.
A thin copper plate is heated to red hot and placed on the top of the threads, then just quickly screw the cap on very tight, the hot copper is quite
soft (much softer than at STP) and molds around the joints to form a perfect seal. I've tested this at 0.001 mmHg and after two hours of being sealed
no noticeable pressure changes were observed. This is ideal for reactive metal distillation as Teflon tape reacts and melts.
-The manipulator
We are all here on earth to help others; what on earth the others are here for I don't know. -W. H. Auden
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Morgan
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Just a tidbit I ran across when reading about 18/10 stainless steel used in the 250ml olive oil bottles I bought. They were $6.99 and just something
to toy with or repurpose maybe.
"18/10' is a designation used on some cutlery and holloware as an alternative to '18/8'. This designation is claimed to indicate a better quality
steel than '18/8', and is essentially the same as the '304 (1.4301) grade . In practice the "10" does not indicate an actual higher Ni content and is
purely a marketing ploy."
http://www.bssa.org.uk/topics.php?article=91
"Chromium and nickel are more expensive than iron. There is a loophole in federal law allowing manufacturers to claim "18/10" if they are at least
8.3% nickel. Many take advantage of this to shave costs, even the high-end brands, so a lot of 18/10 is actually 18/8.3 which is basically 18/8."
http://chowhound.chow.com/topics/926275
 
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Magpie
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Quote: Originally posted by Molecular Manipulations  | I use copper for high temperature and low/high pressure gaskets.
A thin copper plate is heated to red hot and placed on the top of the threads, then just quickly screw the cap on very tight, the hot copper is quite
soft (much softer than at STP) and molds around the joints to form a perfect seal. I've tested this at 0.001 mmHg and after two hours of being sealed
no noticeable pressure changes were observed. This is ideal for reactive metal distillation as Teflon tape reacts and melts. |
Very nice. What thickness plate do you use and what do you use to heat the plate to red hot?
The single most important condition for a successful synthesis is good mixing - Nicodem
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Molecular Manipulations
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I think they're about <s>2-3 mm</s> actually closer to 0.5-1 mm, as I just looked up. About as think as standard
washers. Shows how good I am at approximations (not very). I don't have them at my lab, so I can't measure them now.
I think I used a oxypropane or oxyacetylene torch, either one will do it easily.
[Edited on 20-2-2015 by Molecular Manipulations]
-The manipulator
We are all here on earth to help others; what on earth the others are here for I don't know. -W. H. Auden
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careysub
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There also a variety of metal foils available that might be useful as seals:
http://www.mcmaster.com/#stainless-steel-foil/=vzw53w
http://www.mcmaster.com/#steel-foil/=vzw5dv
Here's a selection of copper washers also:
http://www.mcmaster.com/#standard-copper-washers/=vzw5t7
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violet sin
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http://www.ebay.com/itm/iSi-Cream-Profi-Stainless-Whip-Dispe...
I picked up one of these a while back at a yard sale. I have never used it for anything scientific, but deserts weren't bad. any how, big clunky
stainless with a metal screw on lid. I always thought it might make a good reaction vessel if it wasn't already functioning perfectly as intended.
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Zombie
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| Quote: Originally posted by Molecular Manipulations | I think they're about <s>2-3 mm</s> actually closer to 0.5-1 mm, as I just looked up. About as think as standard
washers. Shows how good I am at approximations (not very). I don't have them at my lab, so I can't measure them now.
I think I used a oxypropane or oxyacetylene torch, either one will do it easily.
[Edited on 20-2-2015 by Molecular Manipulations] |
You can also use a standard propane or mapp gas torch like you get at Ace Hardware or Home centers.
Either has plenty of heat to anneal copper of that gauge. Maybe 20 bucks with the electronic ignite-r tip.
They tried to have me "put to sleep" so I came back to return the favor.
Zom.
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Morgan
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There's these Mason jars made of stainless steel with a silicone gasket - not all that exciting. I recall blowing the lid off one jar having a little
too much confinement with a short length of tubing bolted to the lid and some methanol in the jar, sort of a sustained whoosh bottle attempt. The hole
in the lid was enlarged somewhat by drilling it and adding the length of tubing via some threaded pipe and conduit nuts. Oddly the lid flexed enough
during the "overpressurization" so that the lid still screwed back onto the threads of the jar tightly again without damage. Suffice to say the jar
and single piece lid are very thin steel and if you blow the lid off, it makes a nice bang. ha
http://steelysdrinkware.com/product/steel-mason-jar-30-oz/
And some straws to go with it.
http://www.amazon.com/gp/product/B00AJG5E1U/ref=pd_lpo_sbs_d...
 
[Edited on 22-2-2015 by Morgan]
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Mailinmypocket
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These guys are cute but not exactly cheap:
http://www.qorpak.com/metal-containers/duran-stainless-steel...
Note to self: Tare the damned flask.
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Morgan
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Here's some wine bottles made of stainless steel, kind of different.
http://dgbrilliant.manufacturer.globalsources.com/si/6008844...
http://www.alibaba.com/product-detail/750ml-swing-top-beer-S...
http://www.alibaba.com/product-detail/100ml-1000ml-High-qual...
http://www.alibaba.com/product-detail/no-cap-2-0L-stainless-...
A nice shape here.
http://www.alibaba.com/product-detail/1100ml-stainless-steel...
[Edited on 22-2-2015 by Morgan]
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crazyboy
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I built a pressure vessel like you're talking about. Here are some photos of it.
The yellow stuff is Durham's rock hard putty, it mixes with water to form a paste that gets very hard. That eco canteen was chosen because it's very
cheap. The pressure gauge only goes up to 100 PSI I've taken it past that to the stop which is probably about 150 PSI the bottom bows out but other
than that it's fine.
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j_sum1
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I am going to pinch some of your tubing ideas. I am looking at making a rig for producing my own low pressure gas discharge tubes. I need to control
my vacuum and direct my gases to the right place. Your two valve setup is pretty nifty.
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careysub
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Clearly it is not capable of high temperature operation, with that plastic top, but what temperature have you take it up to (or feel safe with taking
it to)?
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