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US 6,887,947 B1Granted
Synthesis of purified, partially esterified polyol polyester fatty acid compositions
AssigneeThe Procter & Gamble Company
InventorsJared John Schaefer, James Earl Trout
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Abstract
This invention relates to processes for the production of purified, partially esterified polyol fatty acid polyesters and the compositions derived from those processes. The purified, partially esterified polyol fatty acid polyesters of the present invention are particularly well suited for use in a variety of food, beverage, pharmaceutical, and cosmetic applications and comprise less than about 5% polyol; less than about 5 ppm of residual solvent; less than about 700 ppm of lower alky esters; less than about 5% of a soap and free fatty acid mixture; less than about 3% of ash; and have an acid value of less than about 6.
Claims41
A process for the preparation of a purified partially esterified polyol fatty acid polyester composition comprising the steps of:
- a) forming an initial reaction mixture, said initial reaction mixture comprising:
- i) a polyol portion;
- ii) a highly esterified polyol fatty acid polyester;
- iii) a solvent selected from the group consisting of dimethyl formamide, acetonitrile, acetone, and mixtures thereof;
- and
- iv) a catalyst,
- wherein the molar ratio of said polyol portion to said highly esterified polyol polyester is in the range of from about 0.1:1 to about 3:1, wherein the molar ratio of said catalyst to said highly esterified polyol polyester is in the range of from about 0.1:1 to about 40:1, and wherein the weight ratio of said solvent to the combined, weight of said polyol portion, said highly esterified polyol polyester, and said catalyst is in the range of from about 1:1 to about 20:1;
- forming as initial reaction product by reacting said initial reaction mixture in an inert atmosphere, in the presence of a sufficient amount of agitation, for a period of time in the range of from about 30 minutes to about 6 hours, and at a temperature in the range of from about 80° C. to about 140° C.;
- c) optionally drying said initial reaction product;
- wherein in Step (b) agitation is applied at a Weber Number in the range of from about 5000 to about 15000, and for a period of time in the range of from about 30 minutes to about 6 hours.
7 more elements
A process for the preparation of a purified partially esterified polyol fatty acid polyester composition comprising the steps of:
- a) forming an initial reaction mixture, said initial reaction mixture comprising:
- i) a polyol portion;
- ii) a highly esterified polyol fatty acid polyester;
- iii) a solvent;
- and,
- iv) a catalyst,
- wherein the molar ratio of said polyol portion to said highly esterified polyol polyester is in the range of from about 0.1:1 to about 3:1, wherein the molar ratio of said catalyst to said highly esterified polyol polyester is in the range of from about 0.1:1 to about 40:1, and wherein the weight ratio of said solvent to the combined weight of said polyol portion, said highly esterified polyol polyester, and said catalyst is in the range of from about 1:1 to about 20:1;
- b) forming an initial reaction product by reacting said initial reaction mixture in an inert atmosphere, in the presence of a sufficient amount of agitation, for a period of time in the range of from about 30 minutes to about 6 hours, and at a temperature in the range of from about 80° C. to about 140° C.;
- c) adding an acid to the initial reaction product to neutralize any remaining catalyst, wherein the molar ratio of said acid to said catalyst is in the range of from about 0.01:1 to about 1:1;
- d) forming a secondary reaction product by reacting said initial reaction product at a temperature-pressure combination at which distillation of said solvent occurs, wherein the pressure is in the range of from about 0.01 mmHg to about 760 mmHg, for a period of time in the range of from about 30 minutes to about 4 hours;
- e) forming a purified reaction product by washing said secondary reaction product with a solvent free water washing solution, said solvent free water washing solution comprising:
- i) from about 0.1% to about 5% of a salt;
- and
- ii) from about 95% to about 99.9% water;
- wherein the weight ratio of said water washing solution to said secondary reaction product is in the range of from about 3:1 to about 30:1, and wherein the temperature of said secondary reaction product and said water wash solution are in the range of from about 20° C. to about 100° C., wherein said wash time is in the range of from about 5 minutes to about 30 minutes;
- f) isolating and removing impurities from said purified reaction product;
- g) optionally repeating steps (e) and (f) for a number of times in the range of from about 1 to about 20;
- and,
- h) optionally drying said purification reaction product;
- wherein in Step (b) agitation is applied at a Weber Number in the range of from about 5000 to about 15000, and for a period of time in the range of from about 30 minutes to about 6 hours.
17 more elements
A process for the preparation of a purified partially esterified polyol fatty acid polyester composition comprising the steps of:
- a) forming an initial composition comprising the steps of:
- i) a polyol portion;
- ii) a highly esterified polyol fatty acid polyester with a degree of esterification in excess of about 80%;
- iii) a solvent selected from the group consisting of dimethyl formamide, acetonitrile, acetone, and mixtures thereof;
- and,
- iv) a catalyst,
- wherein the molar ratio of said polyol portion to said highly esterified polyol polyester is in the range of from about 0.1:1 to about 3:1, wherein the molar ratio of said catalyst to said highly esterified polyol polyester is in the range of from about 0.1:1 to about 40:1, and wherein the weight ratio of said solvent to the combined weight of said polyol portion, said highly esterified polyol polyester, and said catalyst is in the range of from about 1:1 to about 20:1;
- b) forming an initial reaction product by reacting said initial reaction mixture in an inert atmosphere, in the presence of a sufficient amount of agitation, for a period of time in the range of from about 30 minutes to about 6 hours, and at a temperature in the range of from about 80° C. to about 140° C.;
- c) adding an acid to the inital reaction product to neutralize any remaining catalyst, wherein the molar ratio of said acid to said catalyst is in the range of from about 0.01:1 to about 1:1;
- d) forming a secondary reaction product by reacting said inital reaction product at a temperature-pressure combination at which distillation of said solvent occurs, wherein the pressure is in the range of from about 0.1 mmHg to about 760 mmHg, for a period of time in the range of from about 30 minutes to about 4 hours;
- e) forming a purified reaction product by washing said secondary reaction product with an alcohol washing solution, said alcohol washing solution comprises an alcohol selected from the group consisting of alcohols with a carbon chain length in the range of from about 2 atoms to about 5 atoms, wherein the weight ratio of said alcohol washing solution to said secondary reaction product is in the range of from about 3:1 to about 30:1, and wherein the temperature of said secondary reaction product and said alcohol wash solution are in the range of from about 20° C. to about 100° C., wherein said wash time is in the range of from about 5 minutes to about 30 minutes;
- f) isolating and removing impurities from said purified reaction product;
- g) optionally repeating steps (e) and (f) for a number of times in the range of from about 1 to about 20;
- h) optionally drying said purification reaction product.
11 more elements
Dependencies are inferred from the claim text.