Method for making uniformly-sized particles from insoluble compounds
AssigneeUniversity of Rochester
InventorsMichael R. Violante, Harry W. Fischer
Life of this patent
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Abstract
The invention involves a method for making uniformly sized particles from solid compounds. First, a suitable solid compound is dissolved in a suitable solvent. Then, a precipitating liquid is infused, precipitating non-aggregated particles with substantially uniform mean diameter. The particles are then separated from the solvent. Depending on the solid compound and the desired particle size, the parameters of temperature, ratio of non-solvent to solvent, infusion rate, stir rate, and volume can be varied according to the invention. The precipitating liquid may be aqueous or non-aqueous, depending upon the relative solubility of the compound and the desired suspending vehicle.
Claims22
A method of making uniformly sized particles of a solid compound having an aqueous solubility from about one part per ten thousand to about one part per one hundred, comprising:
- (a) preparing a solution of the solid compound in a suitable solvent for the compound wherein the solubility of the compound in the solvent is greater than about 10 mg/ml;
- (b) infusing a substantially non-aqueous precipitating liquid into the solution at a temperature between about -50.degree. C. and at an infusion rate of from about 0.01 ml per min. to about 3000 ml per min. per 50 ml unit volume of solution, the solid compound having essentially little solubility in the precipitating liquid and the solvent being miscible in the precipitating liquid, so as to produce a suspension of precipitated amorphous, non-crystalline solid compound in the form of substantially non-aggregated particles of a uniform size selected from a particle diameter range of up to about 10 microns, the particle size being directly related to the solution temperature during precipitation and inversely related to the infusion rate;
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- (c) separating the particles from the solvent and washing in a suitable substantially non-aqueous washing liquid, said particles having essentially little solubility in said washing liquid.
A method of making uniformly sized particles of a solid compound having an organic solubility from less than about one part per ten thousand, comprising:
- (a) preparing a solution of the solid compound in an aqueous solvent for the compound, wherein the solubility of the compound in the solvent is greater than about 10 mg/ml;
- (b) infusing a substantially non-aqueous precipitating liquid into the solution at a temperature between about -50.degree. C. and about 100.degree. C. and at an infusion rate of from about 0.01 ml per min. to about 3000 ml per min. per 50 ml unit volume of solution, the solid compound having essentially little solubility in the precipitating liquid and the solvent being miscible in the precipitating liquid, so as to produce a suspension of precipitated amorphous, non-crystalline solid compound in the form of substantially non-aggregated particles of a uniform size selected from a particle of diameter range of up to about 10 microns, the particle size being directly related to the solution temperature during precipitation and inversely related to the infusion rate;
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- (c) separating the particles from the solvent and washing in a substantially non-aqueous washing liquid, said particles having essentially little solubility in said washing liquid.
A method of making uniformly sized particles of a solid inorganic compound, comprising:
- (a) preparing a solution of the compound in a water-miscible solvent for the compounds, wherein the solubility of the compound in the solvent is greater than about 10 mg/ml;
- (b) infusing an aqueous precipitating liquid into the solution at a temperature between about -50.degree. C. and about 100.degree. C. and at an infusion rate of from about 0.01 ml per min. to about 3000 ml per min. per 50 ml unit volume of solution, the solid compound having essentially little solubility in the precipitating liquid and the solvent being miscible in the precipitating liquid, so as to produce a suspension of precipitated amorphous, non-crystalline solid compound in the form of substantially non-aggregated particles of a uniform size selected from a particle diameter range of up to about 10 microns, the particle size being directly related to the solution temperature during precipitation and inversely related to the infusion rate;
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- (c) separating the particles from the solvent and washing in aqueous washing liquid, said particles having essentially little solubility in said washing liquid.
Dependencies are inferred from the claim text.