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US 2003/0229224 A1Published application
Staged 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% by dry weight of polyol; less than about 5 ppm of residual solvent; less than about 700 ppm of lower alky esters; less than about 5% by dry weight of a soap and free fatty acid mixture; and less than about 3% by dry weight of ash. The compositions have an acid value of less than about 6.
Claims44
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 first polyol portion;
- ii) a highly esterified polyol fatty acid polyester;
- iii) a solvent;
- and,
- iv) a catalyst,
- wherein the molar ratio of said first 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 10:1, and wherein the weight ratio of said solvent to the combined weight of said first 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 a secondary reaction mixture, said secondary reaction mixture comprising a second polyol portion, wherein, following the addition of said secondary reaction mixture, the molar ratio of the combination of said first polyol portion and said second polyol portion to said highly esterified polyol polyester is in the range of from about 1:1 to about 40:1;
- d) forming a secondary reaction product by reacting said initial reaction product and said secondary 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 4 hours, and at a temperature in the range of from about 80C to about 140° C.;
- and,
- e) optionally drying said secondary reaction product.
10 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 first polyol portion;
- ii) a highly esterified polyol fatty acid polyester;
- iii) a solvent;
- and,
- iv) a catalyst,
- wherein the molar ratio of said first 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 10:1, and wherein the weight ratio of said solvent to the combined weight of said first 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 a secondary reaction mixture, said secondary reaction mixture comprising a second polyol portion, wherein following the addition of said secondary reaction mixture, the molar ratio of the combination of said first polyol portion and said second polyol portion to said highly esterified polyol polyester is in the range of from about 1:1 to about 40:1;
- d) forming a secondary reaction product by reacting said initial reaction product and said secondary 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 4 hours, and at a temperature in the range of from about 80° C. to about 140° C.;
- e) adding an acid to the secondary 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;
- f) forming a tertiary reaction product by reacting said secondary 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;
- g) forming a purified reaction product by washing said tertiary 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 tertiary reaction product is in the range of from about 3:1 to about 30:1, and wherein the temperature of said tertiary 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;
- h) isolating and removing impurities from said purified reaction product;
- i) optionally repeating steps (g) and (h) for a number of times in the range of from about 1 to about 20;
- and,
- k) optionally drying said purification reaction product.
19 more elements
The process of claim 12 wherein said catalyst is selected from the group consisting of sodium hydride, lithium hydride, potassium hydride, lithium methoxide, potassium methoxide, sodium methoxide, potassium carbonate, sodium carbonate, barium carbonate, and mixtures thereof.
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 first polyol portion;
- ii) a highly esterified polyol fatty acid polyester;
- iii) a solvent;
- and,
- iv) a catalyst,
- wherein the molar ratio of said first 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 10:1, and wherein the weight ratio of said solvent to the combined weight of said first 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 a secondary reaction mixture, said secondary reaction mixture comprising a second polyol portion, wherein following the addition of said secondary reaction mixture, the molar ratio of the combination of said first polyol portion and said second polyol portion to said highly esterified polyol polyester is in the range of from about 1:1 to about 40:1;
- d) forming a secondary reaction product by reacting said initial reaction product and said secondary 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 4 hours, and at a temperature in the range of from about 80° C. to about 140° C.;
- e) adding an acid to the secondary 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;
- f) forming a tertiary reaction product by reacting said secondary 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;
- g) forming a purified reaction product by washing said tertiary 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 tertiary reaction product is in the range of from about 3:1 to about 30:1, and wherein the temperature of said tertiary 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;
- h) isolating and removing impurities from said purified reaction product;
- i) optionally repeating steps (g) and (h) for a number of times in the range of from about 1 to about 20;
- k) optionally drying said purification reaction product.
14 more elements
Dependencies are inferred from the claim text.