Organic compounds -- part of the class 532-570 series – Organic compounds – Carboxylic acids and salts thereof
Patent
1998-02-26
2000-10-24
Richter, Johann
Organic compounds -- part of the class 532-570 series
Organic compounds
Carboxylic acids and salts thereof
C07C 5306
Patent
active
061370053
DESCRIPTION:
BRIEF SUMMARY
The present invention relates to a method for manufacture of products containing disalts of formic acid. The products are manufactured from potassium-, sodium-, ammonium- and cesium-compounds and formic acid containing 0-50% water in a reactor at 40-100.degree. C.
It is often desired to have products with a high concentration of salts of monocarboxylic acids. Such products can be used for several purposes. In formate based animal feed additives, for instance, it is desired that the formate concentration is high and that the product does not emit acids, which act corrosively and may cause poor working conditions during manufacture and handling of the products.
In order to obtain such concentrated products, at least part of the mono salts of said acids can be substituted with disalts like diformate.
The mono salts of potassium, sodium, ammonium and cesium form disalts with monocarboxylic acids like for instance formic acid and acetic acid. The strength of the salt bonds decreases from cesium/potassium to ammonium. Potassium diformates are stable crystalline salts which decompose at temperatures above 120.degree. C. The ammonium diformates are less stable than potassium diformate and the decomposition temperature of ammonium diformate is reported to be in the range 25-30.degree. C. The sodium diformates decompose in the temperature range 100-120.degree. C.
In Gmelins Handbuch der anorganischen Chemie, 8. Ed.System No. 21 and 22, Verlag Chemie G.M.B.H Berlin 1928, pages 81-857 and pages 919-949, respectively there is described formation of disalts of C.sub.1-4 monocarboxylic acids, like potassium diformate and sodium diformate by dissolving pure formates in concentrated and anhydrous formic acid. According to the described laboratory experiments, needle like crystals of diformates etc. are formed. The method for formation of disalts described in Gmelin are only theoretical. Commercial production of such disalts are not reported.
In GB-Patent No. 1.505.388 there is described formation of aqueous solutions of complex salts from ammonium ions and/or ions of a metal selected from Group I and II of the Periodic Table and at least one carboxylic acid. The ratio of acid to ammonium and/or metal ions is in the range of 2:1 and 4:1 on a chemical equivalent basis The concentration of water in the aqueous solution is between 15-75% by weight of the total composition. Said solution of complex salts or disalts of carboxylic acids is stated to be a preservative composition useful in animal feed. This patent does not give any further operating conditions for making the solution of the complex salts and no conditions are given for making dry salts.
The main object of the present invention was to arrive at a new method for the manufacture of products containing disalts of formic acids, where large amounts of the products could be obtained in a form suitable for commercialization.
Another object of the invention was to arrive at products comprising formic acid which were temperature stable i.e. products where the loss of acid was kept at a minimum.
A further object of the invention was to arrive at a crystalline or granulated product which was free-flowing and possessed good storage properties.
Still another object of the invention was to arrive at a product which contains very small amounts of water, and appears with less hygroscopicity compared with the carboxylate itself.
Especially diformates of sodium and potassium were found to have such properties.
It was also an object to produce concentrated solutions or slurries of disalts of formic acid.
By using potassium hydroxide, carbonate, bicarbonate or formate, sodium hydroxide, carbonate, bicarbonate or formate, cesium hydroxide, carbonate, bicarbonate or formate or ammonium formate or ammonia, mixed with formic acid containing 0-30% of water, crystalline diformates were manufactured. The manufactured crystalline diformates were easily separated from the suspension by centrifugation as a filter cake, and the filtrate containing acid salts was collected. The filter cake was tr
REFERENCES:
patent: 1650984 (1927-11-01), Elod et al.
patent: 4261755 (1981-04-01), Berry et al.
Berichte, vol. 36, 1903, E. Groschuff, "Neutral und saure Alkaliformiate. Studien uber die Loslichkeit der Salze, XI" p. 1783-p. 1795.
Gmelins "Handbuch der anorganischen Chemie", 8.Ed System No. 21, Verlag Chemie G.M.B.H. Berlin 1928, pp. 816-819.
Gmelins "Handbuch der anorganischen Chemie", 8.Ed. System No. 22, Verlag Chemie G.M.B.H. Berlin 1928, pp. 919-921.
Kendall et al., "Compound Formation and Solubility in Systems of the Type, Formic Acid: Metal Formate.", Journ. of Am. Chem. Soc. 1921, vol. 43, pp. 1470-1503.
Keys Rosalynd
Norsk Hydro ASA
Richter Johann
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