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Home , Ammonium carbamate

Patented Dec. 10, 1935 2,023,890

UNITED STATES Aren't oFFloE 2,023,890 PRODUCTION 0F METAL ' Ernst Kuss, Marmheim, and Emil Germann, Heidelberg, Germany, assignors to I. G. Far benindustrie Aktiengesellschai’t, Frankfort-on the-Main, Germany, a corporation of Germany No Drawing. Application November 11, 1929, Serial No. 406,510. In Germany December 24, 1928 5 Claims. (01. 260-112) The present invention relates to the production tice, but the invention is not restricted to these of metal carbamates. examples. We have found that metal carbamates, as for Example 1 example , can be obtained in a simple manner from the readily obtainable Sodium chloride is dissolved in liquid . 5 carbamate by bringing the same to A solution of ammonium carbamate in liquid am conversion with inorganic metal compounds, for monia in which further ammonium carbamate example calcium chloride, in inert liquid solvents is suspended is then gradually introduced into capable of dissolving the ammonium carbamate this solution, while stirring, at room tempera 10 and the metal compounds, even if only to a slight ture and under an elevated pressure of about 8 10 extent, that is solvents in which ammonium car atmospheres. Sodium carbamate is precipitated bamate is soluble without the carbamate radical and may be separated from the ammonium chlo su?ering conversion. ride which is dissolved in the liquid ammonia by Alcohols, such as methanol, and other ?ltration. 15 alcohols, and liquid ammonia are for Example 2 15 example suitable as the solvents. According to Calcium chloride is dissolved in ethyl alcohol, the of the ammonium carbamate, which and to this solution a dilute solution of ammonium should be as great as possible, and according to carbamate in ethyl alcohol is gradually added at the solubility of the metal carbamate to be pro a temperature of 50° C. and at ordinary pressure. 20 duced therefrom, which should be as small as Calcium carbamate containing calcium chloride 20 possible, the process is carried out either at or is precipitated. .The remains dinary, high or low temperatures, and accord dissolved in large proportions in the ethyl alco ing to the temperatures employed, at ordinary or hol and is separated from the carbamate by ?l ‘elevated pressures. It is recommended that the tration. By washing the salt with ethyl alcohol 25 conversion be carried out in the absence of wa it is obtained anhydrous. 25 ter. If, however, the solvent has strongly hy groscopic properties, as for example liquid am Example 3 monia, small quantities of water may be pres ent, and this may even be desirable for increasing A solution of ammonium carbamate in meth 30 the solubility of the initial materials. Other anol is added to a suspension of calcium hy- 30 substances, for example those which influence droxide in methanol. The calcium carbamate the solubility of the initial material or the ?nal thus formed is separated from the mother liquor product in a favourable manner, for example am by ?ltration and is converted into calcium cyan monium nitrate in the case of liquid ammonia, amide by heating. 35 may be added to the solvents. Example 4 35 The metal carbamates obtained may then be further worked up into valuable conversion prod Potassium nitrate is dissolved in liquid am ucts. For example calcium carbamate may be monia and a solution of ammonium carbamate in converted into calcium cyanamide or potassium liquid ammonia containing further ammonium 40 carbamate into potassium . carbamate in suspension is then added to this 40 Moreover, without previous separation of the solution. The working temperature is about from metal carbamates, the solvent may be simply re 50° to 70° C. Finely divided ammonium phos moved, for example by evaporation, and in this phate is then added to the mixture. The liquid manner salt mixtures are obtained, in which mix ammonia is allowed to evaporate. The residue 45 tures the metal carbamates may be converted as contains , ammonium ni- 45 hereinbefore described. In this manner for ex trate and potassium carbamate thoroughly mixed. ample valuable mixed can be obtained. Example 5 Further, salts and the like, for example plant To a solution of barium oxide in methanol, in 50 nutrients which are still lacking, may be added before or after the removal of the solvents, espe which further amounts of barium oxide are sus cially when the salt mixtures are to be employed pended, is added a solution of ammonium car as fertilizers. bamate in methanol. It is advantageous to em The following examples will further illustrate ploy ‘an excess of ammonium carbamate over the 55 how this invention may be oazried out in prac barium oxide. Barium carbamate is precipitat- 55 2f 1 2,023,890 ed, which is?separated from the mother liquor compound soluble therein, substantially in the by ?ltration and washed with methanol. absence of water. Example 6 3. The process of producing calcium carba mate, which comprises acting with ammonium A solution of zinc nitratein methanol is slowly carbamate on a calcium salt in an inert liquid added at room temperature and under atmos solvent for-‘the ammonium-carbamate and said pheric pressure to a; solution of ‘ammonium-car calcium‘salt,‘ substantially'in the absence of water. bamate in methanol, While stirring. Zinc car-V 4. The process of producing calcium carba bamate is precipitated, which is ?ltered o? and mate, which comprises acting with ammo 10 washed with methanol and ether. ‘ nium carbamate on calcium chloride in ethyl What we’ claim is:— ' I alcohol, substantially in the absence of water. 1. The process of producing metal carbamates, 5. ‘They process of ‘producing calcium carba Which comprises acting with ammonium carba mate which comprises acting with a dilute solu mate in a monohydric aliphatic alcohol with up to 2 carbon atoms on an inorganic? metal compound’, tion of ammonium carbamate in ethyl alcohol 15 soluble therein, substantially in the absence of on‘ a solution of calcium chloride in ethyl alcohol at ia'temperature' ‘of-50° C.~, substantially in the water. V 7 v ' 2. The process of producing-‘- metal carbamates, absénce'vof Water. which comprises acting with ammonium.carba ERNST KUSS. mate in ethyl alcohol on an inorganicmetal' EMIL GERMANN. 20