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Offline bbmgt3

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TEA problem
« on: March 19, 2014, 08:48:40 AM »
Hi all

So I'm stuck on a work related problem.

I need to come up with a stable solution of triethanolamine 85%, zirconium dichloride oxide, and water.

I can't seem to stop the whole thing from precipitating out.

Appreciate anyone who can offer any suggestions.

Thanks

Offline TheUnassuming

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Re: TEA problem
« Reply #1 on: March 19, 2014, 08:54:33 AM »
Can you give us some more info?  What concentration the zirconyl chloride?  Are you following a published protocol? 
When in doubt, avoid the Stille coupling.

Offline bbmgt3

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Re: TEA problem
« Reply #2 on: March 19, 2014, 10:48:27 AM »
The objective is to achieve a ~3% Zr solution in TEA/Water, so am using 8-9% ZrOxyChloride @ 35% purity.

I am not following a protocol, I'm being asked to come up with one!

Any help would be appreciated.

Offline TheUnassuming

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Re: TEA problem
« Reply #3 on: March 19, 2014, 07:16:33 PM »
Well I haven't used Zr much, but reading a bit more it looks like your reagents when combined are reported for sol formation. So that you are seeing precipitation/colloid formation should be expected.
When in doubt, avoid the Stille coupling.

Offline bbmgt3

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Re: TEA problem
« Reply #4 on: March 20, 2014, 12:41:45 AM »
Right! So, the problem I am facing is what to do or add or some sort of method to prevent this from happening. I know its possible to come up with a stable solution because there are patents out there where you start off with zirconate in propanol but thats real flammable and is undesired.

Any ideas?

Offline TheUnassuming

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Re: TEA problem
« Reply #5 on: March 20, 2014, 03:23:44 PM »
Are you planning on using this around high temp/open flames?
Well it seems like the TEA is probably coordinating the Zr giving you the colloid formation.  If adding propanol forces it into solution then it is most likely coordinating the Zr in one way or another.  You could try other alcohol sources that are less flammable (glycol ect)
When in doubt, avoid the Stille coupling.

Offline bbmgt3

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Re: TEA problem
« Reply #6 on: March 21, 2014, 05:40:38 AM »
Flammability is certainly an issue because it changes the requirements at the plant.

Could you elaborate on the idea of using glycerol? The zirconium is quite readily water soluble at the moment, its the TEA thats the issue. So what mechanism would be at work here?


Offline TheUnassuming

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Re: TEA problem
« Reply #7 on: March 21, 2014, 09:48:05 AM »
Ah, flammability does make a difference at your scale.
So this is the point where I need more information.  Why are you adding the TEA?  What are you trying to accomplish?  What is this going to be used for?
When in doubt, avoid the Stille coupling.

Offline bbmgt3

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Re: TEA problem
« Reply #8 on: March 21, 2014, 11:51:42 AM »
The idea is to have a stable zirconium solution that can be combined with boron compounds and polysaccharides to form cross-linked fluids, controllable by pH sensitivity. So you need TEA or diethylamine to make it work

Offline TheUnassuming

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Re: TEA problem
« Reply #9 on: March 21, 2014, 12:22:38 PM »
Natural gas industry?
So I'm not 100% on the chemistry being done here, so correct me if I'm off course.  Since you need the TEA and you could use propanol if it wasn't so flammable, use a less flammable alcohol.  I'm assuming that the Zr is at least partially complexed by the propanol which allows it to stay in solution.  So perhaps use of something like glycol would work.  PEG (when attached to your molecule) can make a compound much more water soluble, and has a higher viscosity which could be beneficial in your case. 
Have you tried adding in the other reagents to see if it goes in solution?  The hydroxyls on the sugar might also complex the Zr and bring it into solution. 
When in doubt, avoid the Stille coupling.

Offline bbmgt3

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Re: TEA problem
« Reply #10 on: March 21, 2014, 12:53:03 PM »
yes natgas industry! good deduction :)

I will look into it. I have considered looking at other reagents. So where I am is either:

1) Water + TEA + unknown reagent, and then add Zr; maybe at higher temps?
2) Water + Zr + unknown reagent, and then add TEA, again maybe at higher temps.

A glycol is not a bad idea at all, PEG or MEG are readily available and easy to use. The sugars are added later on so they are not part of this process.


Offline Benzene Martini

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Re: TEA problem
« Reply #11 on: March 21, 2014, 08:36:39 PM »
Interesting info. Let us know how it works out.

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