# US 4,394,363 A · Process for the granulation of precipitation products formed from ammonium compounds > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 4,394,363 A - Document ID: US4394363A - Status: Granted - Kind: A - Application number: 06/258,880 - Filed: 1981-04-29 - Granted: 1983-07-19 - Earliest claimed: 1979-07-29 - Assignees: Dr. C. Otto & Comp. G.m.b.H. - Inventors: Egon Haese; Rolf Willms; Karl D. Schultheiss - Web page: https://patentgrep.com/patent/US4394363A ## CPC - C01F 11/00: Compounds of calcium, strontium, or barium (C01F7/00 takes precedence) - C01C 1/10: Separation of ammonia from ammonia liquors, e.g. gas liquors {(as part of the ammonia synthesis process C01C1/04)} - C01F 11/46: Sulfates (dehydration of gypsum {for the production of calcium sulfate cements} C04B11/02) - C01P 2004/50: Agglomerated particles - C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00}) - C01C: AMMONIA; CYANOGEN; COMPOUNDS THEREOF ({metal hydrides, monoborane, diborane or addition complexes thereof C01B6/00}; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; azides C01B21/08; {compounds other than ammonia or cyanogen, containing nitrogen, non-metals and optionally metals C01B21/082}; metal imides or amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; compounds containing silicon C01B33/00; compounds containing boron C01B35/00) - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS ## Abstract A process for the granulation of precipitation products, formed from the reaction of ammonium compounds with alkaline-earth compounds, by introducing into the bottom of a reaction chamber an ammonium and alkaline-earth compound such that the alkaline-earth compound in aqueous solution is immediately and intimately mixed with the ammonium compound to form alkaline-earth compound precipitation products in the form of hard granules which are difficultly soluble in water. The alkaline-earth precipitation products are easily withdrawn from the bottom of the reaction chamber without forming a lime sludge which is difficult to remove. ## Claims ### Claim 1 A process for the granulation of precipitation products formed from the reaction of ammonium compounds with alkaline-earth compounds, which comprises introducing into a liquid-filled reaction chamber above the bottom thereof a first aqueous stream containing the said ammonium compounds and introducing a second aqueous stream containing the said alkaline-earth compounds such that the said alkaline-earth compounds are immediately and intimately mixed with the said ammonium compounds to effect a liquid phase reaction and form alkaline-earth compound precipitation products in the form of granules which are difficultly soluble in water, withdrawing the said granules from the bottom of the said reaction chamber and separately recovering from said reaction chamber a third aqueous stream containing an essentially particle-free aqueous solution of free ammonia and a fourth aqueous stream containing an aqueous solution of free ammonia and suspended particles of said precipitation products. ### Claim 2 (depends on 1) The process of claim 1 including the step of introducing the said first stream and the said second stream separately into the said reaction chamber through a coaxial nozzle assembly. ### Claim 3 (depends on 2) The process of claim 2 wherein said coaxial nozzle assembly introduces said first stream and said second stream into the said reaction chamber tangentially. ### Claim 4 (depends on 1) The process of claim 1 including the step of introducing into the said reaction chamber a fine grained contact substance, disbursed in said second stream, said contact substance selected from the class consisting of quartz, sand and ground calcium carbonate, having a particle size of about 0.2 to 1 millimeter. ### Claim 5 (depends on 1) The process of claim 1 including the step of adjusting the rate of ascent of the liquid in the said reaction chamber such that the resulting granules are kept in a suspended state until they reach a desired size. ### Claim 6 (depends on 1) The process of claim 1 including the step of controlling the flow rate of the said second stream into the said reaction chamber as a function of the pH of the said third aqueous stream.