Sciencemadness Discussion Board

Dissolving titanium metal/dioxide

Hegi - 21-2-2018 at 07:53

Yesterday I went to lab and I was supposed to prepare titanium nitrate for synthesis. I said - no problem - we will just dissolve titanium dioxide in hot concentrated nitric acid. It failed. OK. Then we tried titanium metal. It only dissolved in hot concentrated hydrochloric acid. I thought that oxidizing chloride with HNO3 would replace anions. It worked partially and I got almost clear solution but on heating - titanium dioxide formed. :(

Any ideas how to prepared titanium nitrate?

clearly_not_atara - 21-2-2018 at 08:31

No titanium (IV) binary salts can be obtained from aqueous solution. The lattice enthalpy of TiO2 is much too strong. Anhydrous titanium nitrate is prepared by reacting titanium tetrachloride with dinitrogen pentoxide. It is a volatile, potentially explosive compound.

Titanium (III) nitrate can be prepared in an aqueous solution by salt metathesis, but an inert atmosphere is ideal to prevent oxidation of Ti3+ by oxygen forming TiO2.

Hegi - 21-2-2018 at 11:13

Quote: Originally posted by clearly_not_atara  
No titanium (IV) binary salts can be obtained from aqueous solution. The lattice enthalpy of TiO2 is much too strong. Anhydrous titanium nitrate is prepared by reacting titanium tetrachloride with dinitrogen pentoxide. It is a volatile, potentially explosive compound.

Titanium (III) nitrate can be prepared in an aqueous solution by salt metathesis, but an inert atmosphere is ideal to prevent oxidation of Ti3+ by oxygen forming TiO2.


Thanks a lot for your answer. Yes, after oxidation by nitric acid, formation of TiO2 took place in several seconds. I have never thought about it in this way.

Which salt should be used for metathesis? I think chloride is not suitable because I do not want to have chloride in my system. Inert atmosphere is not a problem.

clearly_not_atara - 21-2-2018 at 13:25

Practically all Ti3+ salts are soluble. Even TiPO4 is soluble IIRC. So any salt can be used, but it must precipitate with the cation of nitrate. Titanium (III) sulfate is a strong contender, undergoing metathesis with calcium nitrate efficiently. If sulfate is also a problem, maybe better luck with titanium (III) bitartrate and potassium nitrate. Although I don't know how to make the bitartrate...

Hegi - 22-2-2018 at 13:51

Quote: Originally posted by clearly_not_atara  
Practically all Ti3+ salts are soluble. Even TiPO4 is soluble IIRC. So any salt can be used, but it must precipitate with the cation of nitrate. Titanium (III) sulfate is a strong contender, undergoing metathesis with calcium nitrate efficiently. If sulfate is also a problem, maybe better luck with titanium (III) bitartrate and potassium nitrate. Although I don't know how to make the bitartrate...


Thanks for another answer... I do not understand clearly your sentence i... it must precipitate with the cation of nitrate? That the product of reaction is the soluble nitrate of titanium and the other salt should be precipitated? If so, I see no problem in CaSO4 formation, I can filter insoluble salt... basically I need to get titanium ion in my Li-Fe-Ti nitrate-glycine oxide synthesis method (if you heard about it). But I dont know how to maintain titanium in Ti3+ state while evaporating water from the mixture. I will have toi take closer look on papers that have been published since date. :)

WangleSpong5000 - 22-2-2018 at 16:23

Titanium dioxide is an adulterant in many hardware store HCl solutions. Fuck knows why... but yeah I spose it must be soluble in 30 + HCl

NEMO-Chemistry - 22-2-2018 at 17:27

Quote: Originally posted by WangleSpong5000  
Titanium dioxide is an adulterant in many hardware store HCl solutions. Fuck knows why... but yeah I spose it must be soluble in 30 + HCl


I might or might not be able to answer that, i will explain how i got the information, it may or may not matter but i am pretty sure it only applies to hardware type grade.

I have a new contact for some chemicals, they are a kind of waste center of sorts. recycle place might be a better description, they take large amounts of industrial used solvents and clean them up.

This is all part of the Scottish zero waste policy thing we have. Anyway I asked why this guys HCl was 1 very cheap, and 2 why was it sometimes pretty crap.

He said it depended on the source for it, he wouldnt say where but he mentioned a place in Newcastle that uses alot of metal. They often get a large amount of HCl off them thats been used as a metal pre wash, it comes in fairly clean compared to what they normally deal with.

They give it a quick clean up and bottle it up and sell on. I am the exception for them, they dont normally deal with the 5ltr guy. But I happen to know him and he dosnt live that far from me...

Only met him a couple of weeks ago, i didnt know the company existed! They called me thinking i was some SME that had started up in the area (my business), and tried selling me solvents by the tanker load!!!

Anyway we had a laugh on the phone and i now have a good source of extremely cheap and contaminated HCl :D.

ninhydric1 - 22-2-2018 at 17:50

While doing research on titanium dioxide nanoparticles I was looking for a way to make TiCl4 from TiO2. I was interested in plante1999's pyrosulfate method where sodium pyrosulfate, sodium chloride, and TiO2 were heated to 400 degrees Celsius IIC to form non-volatile sodium sulfate, while the TiCl4 was distilled off. plante1999 sadly never gave any followup procedure and descriptions, so I didn't delve any deeper. If it does work then TiO2 could be converted to Ti4+ compounds that are actually accessible.

WangleSpong5000 - 22-2-2018 at 18:40

Quote: Originally posted by NEMO-Chemistry  
Quote: Originally posted by WangleSpong5000  
Titanium dioxide is an adulterant in many hardware store HCl solutions. Fuck knows why... but yeah I spose it must be soluble in 30 + HCl


I might or might not be able to answer that, i will explain how i got the information, it may or may not matter but i am pretty sure it only applies to hardware type grade.

I have a new contact for some chemicals, they are a kind of waste center of sorts. recycle place might be a better description, they take large amounts of industrial used solvents and clean them up.

This is all part of the Scottish zero waste policy thing we have. Anyway I asked why this guys HCl was 1 very cheap, and 2 why was it sometimes pretty crap.

He said it depended on the source for it, he wouldnt say where but he mentioned a place in Newcastle that uses alot of metal. They often get a large amount of HCl off them thats been used as a metal pre wash, it comes in fairly clean compared to what they normally deal with.

They give it a quick clean up and bottle it up and sell on. I am the exception for them, they dont normally deal with the 5ltr guy. But I happen to know him and he dosnt live that far from me...

Only met him a couple of weeks ago, i didnt know the company existed! They called me thinking i was some SME that had started up in the area (my business), and tried selling me solvents by the tanker load!!!

Anyway we had a laugh on the phone and i now have a good source of extremely cheap and contaminated HCl :D.


That actually makes perfect sense hey... I never even considered that as a reason.

Are Titanium salts hazardous? I guess it shouldn't be too hard to figure out... heavy metal salts that severely fuck one up permanently usually share a few traits in common: valency (ionic charge... same dif...) plays a role but on its own it may play no role whatsoever. A tendency to bind preferentially to post synaptic receptors essentially permenantly disabling them resulting in the widespread breakodown of neural networks and likely setting off the defence mechanism that destroys the neuron. Ability to attach to the base pairs that DNA and RNA consist of... which causes faults in the codons... enzymes no longer function properly and key biochemical pathways are broken...

And other shit I'm sure...