Dissociation of 1,4-bis (4-phenoxybenzoyl)benzene - lewis acid complex in a protic solvent
US-2019077739-A1 · Mar 14, 2019 · US
US10676418B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10676418-B2 |
| Application number | US-201716330202-A |
| Country | US |
| Kind code | B2 |
| Filing date | Sep 5, 2017 |
| Priority date | Sep 5, 2016 |
| Publication date | Jun 9, 2020 |
| Grant date | Jun 9, 2020 |
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The present invention addresses the problem of providing a method for efficiently producing uniform microparticles of curcumin and/or γ-oryzanol at a higher yield. The target microparticles are produced by dissolving a starting material in a solvent to give a starting material solution and then subjecting the starting material solution to crystallization by a poor solvent method to thereby deposit the starting material. To prepare the starting material solution, curcumin and/or γ-oryzanol are used as the starting material(s) and ethanol is used as the solvent. The starting material(s) and the solvent are stirred in a pressurized state at a temperature of 78.3-130° C. inclusive to give the starting material solution. Then, the starting material solution thus obtained is subjected to crystallization by the poor solvent method and thus the target microparticles are produced.
Opening claim text (preview).
The invention claimed is: 1. A method for producing microparticles, comprising: preparing a raw material solution having a raw material dissolved in a solvent by carrying out a stirring operation of the raw material and the solvent under a pressurized state and a temperature condition of 78.3° C. or higher and 130° C. or lower to produce a pressurized and heated raw material solution, wherein the raw material is at least any one of curcumin and γ-oryzanol; and wherein the solvent is ethanol; holding a pressurized and heated raw material solution at a temperature which is below a standard boiling point of the ethanol; carrying out a crystallization operation by means of a poor solvent method using the pressurized and heated raw material solution thereby obtaining microparticles of at least any one of curcumin and γ-oryzanol. 2. The method for producing microparticles according to claim 1 , wherein the raw material is prepared by carrying out the stirring operation of the raw material solution and the solvent under the pressurized state and the temperature condition not causing boiling thereby obtaining a raw material solution wherein solubility of the raw material to the ethanol is increased. 3. The method for producing microparticles according to claim 1 , wherein when the concentration of curcumin in the raw material solution is taken as x (% by weight), the temperature of a raw material solution to be used in the crystallization operation by means of the poor solvent method is a temperature y (° C.) which is indicated by a formula (1) thereby producing curcumin microparticles y≥ 0.0222 x 3 −2.7 x 2 +30.511 x− 12.833 (1). 4. The method for producing microparticles according to claim 1 , wherein when the concentration of γ-oryzanol in the raw material solution is taken as x (% by weight), the temperature of a raw material solution to be used in the crystallization operation by means of the poor solvent method is a temperature y (° C.) indicated by a formula (2) thereby producing γ-oryzanol microparticles y≥ 0.0762 x 3 −0.9429 x 2 +8.8095 x+ 6×10 −12 (2). 5. The method for producing microparticles according to claim 1 , wherein the average particle diameter of the microparticles is in a range of 30 nm to 1 μm. 6. The method for producing microparticles according to claim 1 , wherein the raw material is selected from the group consisting of ukon, turmeric, a natural extract from ukon, a natural extract from turmeric, a natural extract from rice bran, a natural extract from a corn oil, a natural extract from grains, and mixtures thereof. 7. The method for producing microparticles according to claim 1 , wherein the amount of the microparticles is increased compared to the amount of microparticles produced using a raw material solution that is not prepared under the pressurized state and the temperature condition.
by change in the physical state, e.g. crystallisation · CPC title
with the aid of other complex forming substances than ureum, thioureum or metal salts · CPC title
Use of anti-solvent · CPC title
3 membered carbocyclic rings · CPC title
Dyes of natural origin prepared from natural sources {, e.g. vegetable sources} · CPC title
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