US1835829A - Method for producing titanium compounds and compounds of nitrogen - Google Patents

Description

Patented Dec. 8, 1931 g,ma as moan vonnrcsowsxit, or'or LnNnALn, CALIFORNIA; A ssIGNoa To TITAnIA oonroRA- TION, or LOS anennns, cAmronnIA;A- ooRPonATIon or oALIroamA 5 covery of the nitrogen of the titanium com PATENT OFFICE H 1 METHOD non rnonuome TITANIUM ooiar'ounns oomrounn's' on NITROGEN No Drawing.

The present invention relates to a method for producing titanium compounds and especially to the production of oxygen containing titanium compounds together with the re pounds in the form of combined nitrogen.

I have described, in my United States Letters Patent Number 1,7 42,67 4 dated anuary 7 1930, the preparation of titanium oxide in from titanium nitride by acting upon the latterwith nitric acid. In another pending application for patent Serial No. 320,762 filed November 20th, 1928, I describe the acting upon titanium nitride with nitric acid in the presence of sulphuric acid and show that from this reaction there results titanium acid sulphates. In the practicing of these discoveries, however, only a fraction of the nitride nitrogen of the titanium nitride is recoverable as ammonia or in other combined form.

I have now found that by acting upon tivery good yield, are formed from the nitride nitrogen of the titanium nitride or cyanonitride.

As an example: One heats together titanium nitride and a per cent solution of perchloric acid. Dense fumesare soon given 0E. When the reaction is over the resulting white pasty mass, upon washing with water, gives as a residue titanium dioxidewhile the wash water contains ammonium compounds. The recovery of the nitrogen of the nitride in the form of ammonium perchlorate, ammonium chlorate, etc., is practically quantitative.

As a further example of my discovery: If one warms together titanium nitride and a mixture of diluted sulphuric acid (sp. g. 1.40) and strong perchloric acid (sp. g. 1.5&) in excess of the theory one obtains a solution of Application filed October 30, 1929. Serial No. 403,660.

acid titanium sulphate and. ammonium .sul-

phate. The yields I are nearly quantitative. If desired one may further'dilutesuch a solution, filter, pass in sulphur dioxide, and warm for some hours atabout- 0., whereupon one obtains pure titanium oxide. The solution after filtering off the TiO may be worked up for the recovery of the ammonium compounds present. y I 3 Y If one .uses,'instead of perchloricjacid, a solution of sodium. or calcium hypochlorite in the presence of-hydrochloricacid or even solutions of chlorinein water, either with-or without phosphoric acid-or phosphates, one

canobtain, fro1n-.titaniumnitride, ammonium salts and titanium dioxide One may also use the ha1ates,perhalates or hypohalites of'other alkali or alkaline earth metals... It is further evident that these oxygenated halogensaltslor their acids may be produced: electrolytically in the presence of :titanium nitride, water and a freeacid.

.1. Asan example: If anaqueous solution of sodium chloride, in which is suspended titaniumnitride and containing a little hydrochloric' acid,be electrolyzed, in asuitable cell, one obtains titanium oxide and ammonium salts; -i a I It isto be understood that I do not confine my invention to the examples as given .for they may be modified iby oneskilled in the art without departingfrom the scope of his invention. I I 5:

:What I claim as new and desire to secure by Letters-Patent is:

1.- .Method for the production. of titanium compounds containing oxygen by acting upon titanium nitrogenv compounds with halogen compounds havingv an oxidizing action and in the presence of water and a' free acid and recovering the nitrogenoffthe titanium nitrogen compound in a combined form. r

2.. Method for the production oftitanium compounds containing oxygenand especially titanium acid sulphates by acting upon titanium nitrogen compounds with oxidizing halogen'compounds in the presence ofwater and sulphuric acid and recovering the nitrogenof the titanium nitrogen compound in a. combined form. I

loo

um nitride with by ochlorous acid in the presence of sulphuric acid and water and recovering the nitrogen of the titanium nitride as ammonium sulphate.

12. Method for the production of titanium oxide by acting upon titanium nitride with hypochlorous acid in the presence of water and sodium phosphate.

, FOORD VON BICHOWSKY.

nitrogen-compounds with a hypochlorite of an alkaline metal in the presence of water and a halogen acid andyrecovering the nitrogen of the titanium nitrogen compound as anammonium compound.

' 5. Method forthegproductionof titanium compounds" containing oxygen and especially titanium dioxide by acting upon'titanium nitrogen compounds with "a' chlorate of an alkaline metal in the presence of water and a halogen acid and recovering the nitrogen of the'tita-nium nitrogen compound as an ammonium compound.

'6. 'Method "forlitlie .product-ionof titanium compounds containing'oxygen and especially titanium dioxide by acting upon titanium nit-rogen com-pounds 'with a perchlorate of an alkaline metal in the presence of water and a halogen acid and recovering the'nitrogen of the titanlu-m nitrogen compound asan ammonium compound. I e

7. Method for thepro'duction oftit-anium compounds containing oxygen and especially titanium acid-sulphate by acting upon titan ium nitrogen compounds with hypoc'hlo i v rous acid in the presence of water and sulphuric acid and recovering the nitrogen of the titanium nitrogen compoundas ammonium sulphate. f 3

I '8 Method for the production of titanium compounds containing oxygen and especially titanium acid sulphate by acting upontitanium nitrogen compounds with chloric acid inthe presence of water-and sulphuric acid and recovering the nitrogen of the titanium nitrogen compound as ammonium sulphate.

9. Method for the production of titanium compounds containing oxygen and especially titanium acid sulphate by acting upon titanium nitrogen compounds-with perchloric acidin the presence of water and sulphuric acid'and recovering the nitrogen of the titanium nitrogen compound as ammonium sulphate. 19. Method fortheproduction of titanium compounds containing oxygen and especially sodium titanium acid sulphate by acting upon titanium nitride and sulphuric acidwith an aqueous solution of sodium hypochlorite and "recovering the nitrogen of the titanium ni- -tride'in the form of ammonium sulphate.

11. Methodfor the production of titanium compounds containing oxygen and especially titanium acid sulphate by acting upon titani-