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(12) United States Patent (10) Patent No.: US 7.462,342 B2 Tomiyama Et Al

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(12) United States Patent (10) Patent No.: US 7.462,342 B2 Tomiyama Et Al USOO7462342B2 (12) United States Patent (10) Patent No.: US 7.462,342 B2 Tomiyama et al. (45) Date of Patent: Dec. 9, 2008 (54) METHOD FOR PRODUCING BASIC METAL (56) References Cited NITRATE U.S. PATENT DOCUMENTS (75) Inventors: Shogo Tomiyama, Hyogo (JP); Xingxi 3,983,221 A * 9, 1976 Rademachers et al. ...... 423,395 4,136,157 A * 1/1979 Asai et al. ... ... 423.395 Zhou, Hyogo (JP) 5,000,928 A * 3/1991 White ....... ... 423/34 5,039,502 A * 8/1991 Hornet al. ........ ... 423.395 (73) Assignee: Daicel Chemical Industries, Ltd., 5,429,691 A * 7/1995 Hinshaw et al. ............... 149/45 Sakai-Shi (JP) 6,468.494 B2 * 10/2002 Nappier et al. .............. 423,395 2007/01 19530 A1 5/2007 Zhou et al. *) NotOt1Ce: Subjubject to anyy d1Sclaimer,disclai theh term off thisthi patent is extended or adjusted under 35 FOREIGN PATENT DOCUMENTS U.S.C. 154(b) by 772 days. EP 1241 138 A1 9, 2002 (21) Appl. No.: 10/468,039 (Continued) (22) PCT Filed: Mar. 27, 2002 OTHER PUBLICATIONS (86). PCT No.: PCT/UP02/03005 Gmelins Handbuch Deranorganischen chemie “kuper Teil B. pp. 188-193, 1958 (corresponds to specification p. 1, line 10, no month. S371 (c)(1), (2), (4) Date: Feb. 17, 2004 (Continued) Primary Examiner Wayne Langel (87) PCT Pub. No.: WO02/079091 (74) Attorney, Agent, or Firm—Birch, Stewart, Kolasch & Birch, LLP PCT Pub. Date: Oct. 10, 2002 (57) ABSTRACT (65) Prior Publication Data US 2004/O131529 A1 Jul. 8, 2004 A process in which a basic metal nitrate is obtained in a high yield is provided. (30) Foreign Application Priority Data A process for producing a basic metal nitrate, which com Mar. 29, 2001 (JP) ............................. 2001-094976 prises adding an aqueous solution of a metal nitrate or an aqueous Solution of a mixture of a metal nitrate and a water (51) Int. Cl. soluble additive and an alkali solution to a reaction vessel in COIB 2L/248 (2006.01) which a reaction solvent whose pH at 20°C. is adjusted to 6 (52) U.S. Cl. ...................................................... 423A395 or less is present, and conducting the reaction with stirring. (58) Field of Classification Search. ... 423 (395 See application file for complete search history. 12 Claims, 2 Drawing Sheets US 7.462.342 B2 Page 2 FOREIGN PATENT DOCUMENTS OTHER PUBLICATIONS JP 57-209822 12/1982 ............. ... 423.395 Acta Chemica Scandinavia A 30, No. 5. 343-350 (corresponds to JP 60-200825 A 10, 1985 specification at p. 2, line 2, no date. JP O2-145422 A 6, 1990 Aust. J. Chem., 1990,42, pp. 749-754 (corresponds to specification at JP O2-204321 A 8, 1990 p. 2, line 9, no month. JP O7-187673 A 7, 1995 * cited by examiner U.S. Patent Dec. 9, 2008 Sheet 1 of 2 US 7.462,342 B2 sers is: 'ti-air U.S. Patent US 7.462,342 B2 Fig. 2 03||000/06080Z |eIduIexGI–?— a- -- a------------------------------ a sea are r is an on 4 mm mm. Frrera's r mawr wave --------------------s-s-- - - - - ------- 90 --------------a-a-as-- a--------a-on G as a ran arm manasma same a sara or m in a maid as arra aaa-arm r - - - -- a ------------------------------------------ as-s-s-su in a -- as sasss: S OŽ0||0 t O O 00‘Z 00,9 O US 7.462,342 B2 1. 2 METHOD FOR PRODUCING BASIC METAL before starting a reaction is adjusted to between 1.5 and 2.5 is NITRATE present, and conducting the reaction with stirring through a stirring unit so that the maximum pH value reaches 5.0 to 6.5 This application is the national phase under 35 U.S.C. 371 during the reaction. of PCT International Application No. PCT/JPO2/03005 5 The pH is determined depending on various factors to be which has an International filing date of Mar. 27, 2002, which described below, and is adjusted by properly selecting the designated the United States of America. respective factors. The basic metal nitrate obtained by the process of the TECHNICAL FIELD TO WHICH THE invention includes compounds represented by the following INVENTION BELONGS 10 general formula (I), and some compounds contain hydrates tOO. The present invention relates to a process for producing a basic metal nitrate. M(NOs), nM(OH), or M, (NO3)(OH), (I) PRIOR ART wherein M represents a metal, x' represents the number of 15 metals, y and y each represent the number of NO ions, z' With respect to a process for producing a basic metal represents the number of OH ions, and n represents a ratio of nitrate, various processes have been so far known. For an M(OH), moiety to an M(NO), moiety. example, as a process for producing a basic copper nitrate Examples of the compounds corresponding to the general using a copper nitrate solution, a process described in GME formula (I) include those containing, as a metal M. copper, LINS HANDBUCH DERANORGANISCHEN CHEMIE cobalt, Zinc, manganese, iron, molybdenum, bismuth and “KUPFER Teil B, pp. 188-193 (System Number 60), 1958; cerium, Such as basic copper nitrates Cu2(NO)(OH) and VERLAG CHEMIE, GMBH. WEINHEIM/BERG Cu(NO) (OH).2H2O), basic cobalt nitrate CO(NO) STRASSE is known. In this literature, a process using a (OH), basic Zinc nitrate Zn (NO)(OH), basic manga copper nitrate Solution and ammonia oran alkali hydroxide, a 25 nese nitrate Mn(NO)(OH), basic iron nitrate Fe(NO) reaction of a dilute copper nitrate aqueous solution with a 0.1 (OH).2H2O), basic molybdenum nitrate, basic bismuth NSodium hydroxide aqueous Solution, a reaction of a neutral nitrate Bi(NO)(OH) and basic cerium nitrate Ce(NO) copper nitrate Solution with a sodium hydroxide aqueous (OH).3H2O. Of these, basic copper nitrates (BCN) are pref Solution, a reaction with ammonium nitrate in the presence of erable. air and water and the like are described as a process for 30 According to the process of the invention, a basic metal producing a basic copper nitrate. However, in all of these nitrate Such as a basic copper nitrate or the like can industri processes, a yield of a basic copper nitrate is unclear, and ally be produced using a starting material which is less costly further a color and a crystalline state of the resulting basic and can be procured industrially easily without the special copper nitrate are not fixed. Thus, it is difficult to utilize the need of a special reaction equipment and under readily con same industrially. 35 trollable reaction conditions. Further, a basic metal nitrate in Acta Chemica Scandinavia A 30 No. 5 343-350 (1976) fixed crystal form having a uniform particle diameter (narrow describes a process with a copper nitrate solution-ammo particle size distribution) can be obtained in a high yield. nium nitrate Solution-aqueous ammonia system. However, Moreover, when the basic metal nitrate obtained by the although the production is conducted using a 4-liter flask in process of the invention is used as an oxidizing agent of a gas this process, an amount is as Small as 5 g. When this is 40 generating agent for an inflator, a burning rate of the gas calculated on a plant Scale, the yield is as low as approxi generating agent can be adjusted to a preferable range. mately 53%. Thus, it is difficult to utilize the same industri ally. BRIEF DESCRIPTION OF DRAWINGS In Aust. J. Chem., 1990, 43, 749-754, it is described that when a 10' M potassium hydroxide solution is gradually 45 FIG. 1 is a conceptual view for describing a process of the added to a solution in which a concentration of a divalent invention. copper ion in a copper nitrate solution is 10 or 10 Mand FIG. 2 is a graph showing a change in pH of a reaction a concentration of a nitrate anion by potassium nitrate is 10, system with time. 10° or 10 M, a pH value at the initial stage of the solution MODE FOR CARRYING OUT THE INVENTION is adjusted to approximately 3. This process is, however, 50 problematic in that since it includes a step of using a dilute Solution, a production time is more than approximately 36 One embodiment of the process of the invention is hours and too long. described below according to production steps. However, the following production steps can undergo changes and addi DISCLOSURE OF THE INVENTION 55 tions, as required, by modifications which are commonly conducted by those skilled in the art. The object of the invention is to provide a process for First, an aqueous solution of a metal nitrate or an aqueous producing a basic metal nitrate in which a high-quality basic solution of a mixture of a metal nitrate and a water-soluble metal nitrate is obtained in a highyield and at good efficiency, additive which is a reaction starting material and an aqueous and to provide a basic metal nitrate which is composed in 60 Solution of an alkali are prepared. accordance with the above process. The metal nitrate is preferably a metal salt of at least one The invention provides, as a means for Solving the prob metal selected from cobalt, copper, Zinc, manganese, iron, lem, a process for producing a basic metal nitrate, which molybdenum, bismuth and cerium. Copper nitrate is more comprises adding an aqueous Solution of a metal nitrate oran preferable. aqueous Solution of a mixture of a metal nitrate and a water 65 The water-soluble additive is at least one selected from soluble additive and an aqueous Solution of an alkali to a ammonium nitrate, ammonium nitrite, ammonium acetate, reaction vessel in which a reaction solvent whose pH (20°C.) ammonium carbonate, ammonium bicarbonate, ammonium US 7.462,342 B2 3 4 Sulfate, ammonium sulfite, ammonium bisulfate, ammonium SfS is too high, the reaction system cannot be rendered bisulfite, ammonium hydrogensulfate, ammonium hydrogen uniform.
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