| CPC C05F 3/00 (2013.01) [C05C 3/00 (2013.01); C05D 9/00 (2013.01); C07F 9/28 (2013.01)] | 20 Claims |
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1. A method to make one or more alkyl thiophosphoric triamides, comprises:
a) a Step One, wherein a first reactant is reacted with a second reactant within a reaction medium and in the presence of a first hydrochloric acid neutralizer (HAN-1), wherein the Step One comprises:
i. the first reactant, the HAN-1 and the reaction medium are charged to reactor 1 and is cooled to a temperature range of (−40° C.) to 0° C., wherein the first reactant comprises thiophosphoryl chloride,
ii. the second reactant is optionally diluted with the reaction medium and optionally cooled to a temperature range of (−40° C.) to 0° C., wherein the second reactant is one or more mono-alkyl amines,
iii. slowly charging the second reactant subsurface of the reactor 1's contents, wherein the first reactant reacts with the second reactant generating a strong exotherm, wherein agitation is used to prevent localized high temperatures generated by the reaction exotherm, and maintaining batch temperature at a range of (−40° C.) to 0° C.,
iv. after completing the charge of the second reactant, the contents are mixed until all the second reactant is consumed resulting in a composition comprising, a) a first adduct, and b) one or more HAN-1 chloride salts, and
b) a Step Two, wherein the Step Two comprises:
i. a third reactant is slowly charged above the surface of the contents of the reactor 1 and/or below the surface of the contents of the reactor 1, wherein the contents of reactor 1 are maintained at a temperature range of (−20° C.) to 50° C.,
ii. wherein the third reactant is charged and reacted until no residual phosphoryl chlorides are present in the contents of reactor 1 and results in a second adduct, wherein the second adduct comprises the one or more alkyl thiophosphic triamides,
iii. wherein optionally a second hydrochloric acid neutralizer (HAN-2) is charged to the contents of the reactor 1, and
iv. wherein the chloride salts are removed from the reactor 1 contents by one or more techniques selected from the group consisting of (1) breaking a fused binary particle and filtering out the chloride salts and (2) washing out the chloride salts by dissolving them in water or optionally in a water with a pH adjusted with ammonium hydroxide, wherein the fused binary particle composition comprises chloride salts and the one or more alkyl thiophophoric triamides,
c) a Step Three, wherein the Step Three comprises:
i. a solution of one or more alkyl thiophosphoric triamides dissolved in the reaction medium is collected, and
ii. a solvent exchange is implemented wherein the components of the reaction medium with a boiling point of about 120° C. or less are displaced by a Solvent System Two to form a non-aqueous organic liquid delivery system for delivering the one or more alkyl thiophosphoric triamides to the surface of one or more nitrogen fertilizers granules, wherein Solvent System Two comprises one or more solvents selected for the group consisting of a) one or more additional aprotic organic liquids and b) one or more protic organic liquids and wherein the non-aqueous organic liquid delivery system comprises the following properties:
(1) are environmentally safe,
(2) having a flashpoint above 145° F.,
(3) are rated safe for contact with humans and animals,
(4) having % loading of one or more alkyl thiophosphoric triamides of 20-95%,
(5) are fluid at temperature range of −20 to 100° C.,
(6) can be applied to the one or more nitrogen fertilizer granules through application by commercial sprayers and metered applicators onto fertilizer granules mobilized by mixing, stirring and/or blending to ensure an even coating of the solution of alkyl thiophosphoric triamide on the surfaces of said nitrogen fertilizer granules through commingling of said solution with said nitrogen fertilizer granules.
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