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United States Patent Office Patented Mar. 15, 1938 ' " UNITED STATES PATENT OFFICE 2,111,460 ALKALI METAL TITANATES Joachim Rockstroh, Cologne-Deutz, Germany, as Signor, by mesne assignments, to National Lead Company, New York, N. Y., a. corporation of New Jersey No Drawing. Application July 14, 1934, Serial No. 735,289. In Germany August 22, 1933 7 Claims. (Cl. 23-51) This invention relates to the manufacture of ployed for the manufacture of other titanium alkali metal titanates by heating titanium oxygen compounds, for instance, organic titanium com compounds with alkalies, more particularly it pounds, since contaminations of ‘these com relates to subjecting dry and pulverized mix- pounds, for instance of alkali metal titanium 5 tures of titanium oxygen compounds and alka- oxalic acid solutions with alkali metal sulfate, 5 lies to heat treatment below the melting point are thus avoided. , of the alkali employed. The process can be carried out in such a man Alkali metal titanates may be produced by ner that dried meta titanic acid or calcined ti heating titanium dioxide with alkali metal hy- tanium dioxide is intimately mixed with dry '10 droxides or alkali metal carbonates to tempera- powdery alkali metal hydroxide or oxide and is 10 tures of GOO-700° C. It is known that the manu- heated to the appropriate temperature in a re facture of alkali metal titanates can also be per- action vessel suitable for this purpose, for in formed at lower temperatures of 80—200° C., if stance, in an iron pan which may be provided hydrated titanium oxygen compounds are heated with a stirrer. The temperature most favorable 15 with alkalies. In this process a paste made of for carrying out the process is from about 150° 15 hydrated titanic acid and water and containing to about 220° C., but also lower or higher temper 30% of TiOz is produced, the mixture is treated atures up to below the melting point of the alkali with the necessary quantity of alkali metal car- metal hydroxide or oxide may be employed. The bonate or hydroxide and heated to a tempera- higher the temperature the more rapidly the re 20 ture of between 80 and 200° C. The water there- action is complete and the higher rises the con- 20 by evaporates. The products thus obtained al- tent of titanium of the product within certain ways contain alkali metal sulfates because the ranges, since the technical alkali metal hydrox hydrated meta titanic acids obtained from 171- ide or oxide always contains a certain quantity tanium sulfate solutions by the known methods of water which evaporates during the heating 25 always contain some sulfate. process. Besides this, the quantity of water 25 In accordance with1 the present invention it formed according to the equation has been found that t e formation of alkali metal . titanates readily occurs on intimately mixing T102+2K0H=K2T1O3+H20 dry titanic acid and solid alkali metal hydroxide must be taken into consideration. The alkali 30 or oxide and heating the mixture to a tempera- metal hydroxide or oxide may be applied in such 30 ' ture of about 150-220° C. This process offers quantities that meta titanates of the formula many advantages because no evaporation of a MezTiOs are formed. But also smaller quantities large quantity of Water necessary for carrying of alkali may be applied so that products of a out the process in accordance with the known higher TiOz content are formed. When produc 35 methods takes place. Thus no waste of energy ing sodium titanate a slight excess of sodium 35 occurs. Further, it is known that an aqueous hydroxide or oxide is preferred since, as is known, paste of titanic acid hydrate and alkali metal the action of sodium hydroxide on titanium oxy hydroxide on heating and drying tends to spray gen compounds is not as strong as the action of and thereby endangers the workmen. This dis- potassium hydroxide or oxide on titanium oxy 40 advantage is overcome by the new process. gen compounds. In the same manner also 40 Further, it has been found that not only dried caesium, rubidium and lithium titanates may be titanic acid without the addition of water reacts produced. After the heat treatment the prod with alkali metal hydroxide at moderately high uct may be ground with or without additions or temperatures with the formation of alkali metal it may be used directly for the manufacture of 45 titanates, but also that calcined titanium dioxide other titanium compounds. 45 can be converted into alkali metal titanate in The invention is further illustrated by the fol the same manner. This is surprising since, as lowing example: is known, the reactivity of titanic acid is greatly ExampZe.-—500 parts by weight of titanium di reduced by calcining. A great advantage of the oxide, produced from hydrolytically precipitated 50 new process is to be seen therein that it becomes meta titanic acid by heating for one hour to 50 possible to use titanium dioxide which by calcin- 950° C. and which contains no sulfate, are inti ing has been completely liberated from sulfuric mately mixed with 750 parts by weight of techni acid, so that titanates free from alkali metal cal, powdery potassium hydroxide and heated ina' sulfate can be produced. This is of especial ad- drier for about three quarters of an hour to 55 vantage if the alkali metal titanate is to be em- ISO-170° C. The white product consists of 55 2 2,111,460 K2TlO3 which is soluble in cold hydrochloric 4. The process of preparing an alkali metal acid and contains a small amount of insoluble titanate which comprises intimately mixing dry residue (T102) . It is free from sulfate. and pulverized arti?cially prepared titanium The expressions “oxygen compound of titan dioxide with dry and pulverized potassium hy ium” and “oxygen compound of an alkali metal” droxide and heating the mixture so obtained at used in the claims are intended to comprise the temperatures between about 150° C. and 220° C. oxides as well as the hydroxides of titanium and until formation of the alkali titanate is substan the alkali metals. tially complete. I claim:—— 5. The process of preparing an alkali metal 10 1. The process of preparing an alkali metal titanate which comprises intimately mixing dry titanate, which comprises intimately mixing a and pulverized arti?cially prepared meta-titanic dry and pulverized arti?cially prepared titanium acid with dry and pulverized potassium hydrox oxygen compound with a dry and pulverized ide and heating the mixture so obtained at tem oxygen compound of an alkali metal and heat peratures between about 150° C. and 220° C. un 15 ing the mixture so obtained to a temperature til formation of the alkali titanate is substan 15 of about 150° C. to 220° C‘. until formation of tially complete. alkali metal titanate is substantially complete. 6. The process of preparing an alkali metal 2. The process of preparing an alkali metal titanate which comprises intimately mixing dry titanate, which comprises intimately mixing dry and pulverized arti?cially prepared titanium 20 and pulverized arti?cially prepared titanium dioxide with dry and pulverized sodium hydroxide 20 dioxide with a dry and pulverized oxygen com and heating the mixture so obtained at tem pound of an alkali metal and heating the mix peratures between about 150° C‘. and 220° C. un ture so obtained to a temperature of about 150° til formation of the alkali titanate is substan C. to 220° C. until formation of alkali metal tially complete. 1 25 titanate is substantially complete. '7. The process of preparing an alkali metal 25 3. The process of preparing an alkali metal titanate which comprises intimately mixing dry titanate which comprises intimately mixing dry and pulverized arti?cially prepared meta-titanic and pulverized arti?cially prepared meta-titanic acid with dry and pulverized sodium hydroxide acid with a dry and pulverized oxygen compound and heating the mixture. so obtained at tempera 30 of an alkali metal and heating the mixture so tures between about 150° C. and 220° C. until 30 obtained at temperatures between about 150° C. formation of the alkali titanate is substantially and 220° C. until formation of the alkali titanate complete. is substantially complete. JOACHIM ROCKSTROH. .
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