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(12) United States Patent (10) Patent No.: US 6,365,120 B1 Granquist Et Al

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(12) United States Patent (10) Patent No.: US 6,365,120 B1 Granquist Et Al USOO636512OB1 (12) United States Patent (10) Patent No.: US 6,365,120 B1 Granquist et al. (45) Date of Patent: Apr. 2, 2002 (54) METHOD FOR HARDENING GRANULAR 3,485,580 A 12/1969 Mischel et al. NORGANIC SALT COMPOUNDS 3,640,697 A * 2/1972 Toops, Jr. ................... 423/396 4.326,976 A * 4/1982 Logan et al. ............... 252/383 (75) Inventors: Victor Martin Granquist; Robert Paul 4,717,555 A * 1/1988 Newman et al. ............ 423/396 Kern, Jr., both of Beaufort, SC (US) 6,022,386 A * 2/2000 Vogel et al. ................ 423/396 (73) Assignee: (US)Lobeco Products, Inc., Lobeco, SC FOREIGN PATENT DOCUMENTS (*) Notice: Subject to any disclaimer, the term of this PL 86493 1/1924 patent is extended or adjusted under 35 PL 120497 12/1978 U.S.C. 154(b) by 0 days. * cited by examiner (21) Appl. No.: 09/514,277 (22) Filed: Feb. 28, 2000 Primary Examiner Wayne Langel (51) Int. Cl. .............................. Co1C 1/18, CosG 500 (74) Attorney, Agent, or Firm-Robert C. Brown (52) U.S. Cl. ............................... 423/268; 71/34; 71/58; (57) ABSTRACT 71/64.12; 252/383; 423/396 (58) Field of Search ................................ 71/34, 58, 61, Solid inorganic particulate Salts having increased hardneSS 71/64.12; 423/268, 396; 252/383 are produced by incorporating a novel additive composition (56) References Cited comprised of ammonium Sulfate and a naphthalene Sulfonate compound. U.S. PATENT DOCUMENTS 3,230,038 A 1/1966 Wilson ....................... 423/268 13 Claims, No Drawings US 6,365,120 B1 1 2 METHOD FOR HARDENING GRANULAR with Said mixture by introducing an aqueous Solution of NORGANIC SALT COMPOUNDS ammonium Sulfate and a naphthalene Sulfonate into the melt liquor of the inorganic Salt. FIELD OF THE INVENTION DETAILED DESCRIPTION OF THE This invention relates to a method of hardening prills and INVENTION granules of inorganic Salt compounds to reduce clumping Illustrative of the inorganic Salt compounds which can and powder and dust formation. benefit from the invention are ammonium nitrate, di-ammonium phosphate, mono-ammonium phosphate, BACKGROUND OF THE INVENTION potassium nitrate, potash and complex fertilizer composi tions. The invention is especially useful for the manufacture A variety of inorganic Salt compositions find extensive of fertilizer grade ammonium nitrate having Superior hard use in agriculture as well as in other applications. Examples neSS and Stability properties. of inorganic Salt compounds which are used for Such pur The advantages achieved by the practice of this invention poses include ammonium nitrate, di-ammonium phosphate, derive from the dramatic improvement in the physical mono-ammonium phosphate, potassium nitrate, potash 15 properties of inorganic Salt granules and prills which result (potassium carbonate and potassium chloride) and various from the introduction of a novel hardening mixture, com other inorganic Salts. prising a naphthalene Sulfonate compound and ammonium To prevent caking and clumping and to obtain other Sulfate, into the inorganic Salt. This novel mixture is a used desirable physical properties, it is customary to coat or in the form of an aqueous mixture of ammonium Sulfate and otherwise modify these materials with one or more of a one or more naphthalene Sulfonate compounds of the for variety of different internal additives. Illustrative of these mula (including dimers and trimers thereof): materials are magnesium oxide, various clays and mixtures of a variety of different inorganic salts. While these materials impart Some beneficial properties, their use for these pur poses has Some Serious disadvantages. For example, while 25 magnesium oxide when applied to ammonium nitrate par (R). ticulate improves hardneSS and Stability, it is difficult to apply as it must be metered and handled as a solid. When incorporated in ammonium Salts, magnesium oxide can also wherein M is ammonium or an alkali or alkaline earth metal; cause an undesirable release of ammonia. The application of each R is independently, hydrogen or an alkyl Substituent magnesium oxide to inorganic Salts can also result in having from 1 to 12 carbon atoms, X is a whole number of increased hygroscopicity which may increase the likelihood from one to Seven; and y is a whole number of from one to of clumping and agglomeration which is highly undesirable. two with the provisos that the total number of carbon atoms Clay additives also present handling problems, due to contained in all of the R groups combined may not exceed their insolubility, which makes it necessary to handle them 35 16 and the Sum of X and y may not exceed eight. Illustrative as Solids and in the usual case, disperse them with difficulty, of the useful naphthalene Sulfonate compounds are Sodium in the melt liquor used to produce the Solid prill or granule 1-methylnaphthalene Sulfonate, potassium 1-methyl-3- of the inorganic Salt being treated. Because they are inert and methylnaphthale n e Sulfonate, potassium must be used in Significant amounts, they also degrade the 1- is op ropylnaphthale n e Sulfonate, calcium 40 4-ethylnaphthalene Sulfonate as well as dimers, trimers and efficacy of the product because of dilution. Most of these mixtures thereof. The useful naphthalene Sulfonate com modifiers also have an undesirable effect on the color of the pounds are easily prepared by Sulfonation of naphthalene or product an appropriately alkylated naphthalene compound followed Most inorganic Salt mixtures used as modifiers for inor by neutralization with ammonium hydroxide or an alkali or ganic Salts tend to be expensive, yield inconsistent results 45 alkaline earth metal hydroxide compound. The addition of and require relatively high concentrations to be effective, formaldehyde to the reaction mixture after Sulfonation and thereby adversely affecting performance of the product, due before neutralization will yield the dimer or trimer form of to the effect of dilution. For example, ammonium Sulfate is the naphthalene Sulfonate compound. The hardening mix a well known hardening (anti-clumping and anti-dusting) ture is preferably employed in an amount Such that it will be agent for ammonium nitrate. Unfortunately it must be 50 present in an amount equal to between 0.05 percent to about present in an amount of at least about 2% by weight of the 0.2 percent of the total weight of the final salt product. total final composition to be effective. It also presents. Some It has also been found that by adding one or more optional very difficult manufacturing problems due to a necessity to alkali or alkaline earth metal benzene Sulfonate compounds, form the Sulfate Salt in Situ during the manufacturing pro which may have one or more alkyl Substituents containing a CCSS. 55 total number of carbon atoms between three and 12, further improvements in the physical properties of the inorganic Salt SUMMARY OF THE INVENTION compound can be achieved. Illustrative of the useful It has now been found that the use of a mixture of optional alkyl benzene Sulfonate compounds are Sodium ammonium Sulfate with certain naphthalene Sulfonates (the isopropylbenzene Sulfonate, ammonium isopropylbenzene expression “naphthalene Sulfonate” as used herein includes 60 Sulfonate, potassium di-isopropyl benzene Sulfonate, mag dimerS and trimers of the described class of naphthalene nesium Xylene Sulfonate, calcium 2-methyl-4-isopropyl Sulfonates as well as monomeric naphthalene Sulfonates) for benzene Sulfonate, Sodium butylbenzene Sulfonate, ammo improving the physical properties of inorganic Salt granules nium di-butylbenzene Sulfonate, potassium hexyl benzene and prills produces an unexpected and Synergistic improve Sulfonate, Sodium octylbenzene Sulfonate and Sodium dode ment in the physical properties of these materials. This 65 cylbenzene Sulfonate. invention also is directed to a proceSS for preparing Said The novel hardening additive of this invention is prepared mixture and for hardening inorganic Salt granules and prills by first dissolving a naphthalene Sulfonate compound in US 6,365,120 B1 3 4 water at a concentration of from about one percent to about EXAMPLES 50 percent by weight. Ammonium sulfate is then added to the Solution in an amount equal to from about 10 percent to Example 1 about 70 percent by weight of the final solution. The optional benzene Sulfonate compound may also be added at this time in an amount ranging from about one percent to about five Preparation of Samples for Evaluation percent by weight of the Solution. Wafer Method In a typical commercial production of Solid inorganic Salt Measured amounts of additive composition with a 25.0 prills or granules, using ammonium nitrate as an example, gram Sample of ammonium nitrate and melted at a tempera nitric acid and anhydrous ammonia are reacted together in a 1O ture of 170 to 175 C. in a covered beaker in a forced draft neutralizer to produce a slightly acid aqueous Solution of oven. The resultant liquid melt was stirred to ensure com ammonium nitrate at a concentration of about 82 to 83 plete mixing with the additive composition and the further percent by weight. It is preferred to incorporate the novel heated to achieve and maintain a temperature of from 170 hardening additive of this invention into the inorganic Salt to 175 C. The sample was then removed from the oven and compound melt at this stage. This is easily accomplished by 15 poured into an aluminum weighing dish of 70 mm diameter the simple expedient of introducing the liquid additive positioned on a level Surface and then covered with foil. mixture into a melt liquor of the inorganic Salt. The amount added should be sufficient to produce an amount of the Neat samples of ammonium nitrate without the novel addi non-aqueous component of the additive equal, preferably, to tive of the invention were prepared in the identical manner. from about 0.05 percent to about 0.2 percent by weight of After cooling for at least two hours the Samples were then the final inorganic Salt product.
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