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Claims for Patent: 5,441,738

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Claims for Patent: 5,441,738

Title: Process for improving a glycerolysed oil
Abstract:There is disclosed a process for improving a glycerolyzed oil. The oil is heated until any crystals which have formed have disappeared. Then the oil is crystallized by slow stirring for eight to seventy-two hours until an end of crystallization temperature of typically between 0.degree. and 15.degree. is reached. Finally the crystals which have formed are separated at the end of crystallization temperature. The process can be iterated at two successively lower end of crystallization temperatures.
Inventor(s): Klein; Jean-Marie (Feyzin, FR), Denis; Joel (Vourles, FR)
Assignee: Gattefosse SA (FR)
Application Number:08/081,355
Patent Claims: 1. A process of preparing a fractionated glycerolyzed oil having improved crystallization stability, consisting essentially of the steps of:

heating the glycerolyzed oil to a temperature of about 80.degree. C. and maintaining the glycerolyzed oil at said temperature until crystals are absent therein, the glycerolyzed oil being richer in monoglycerides and diglycerides than in triglycerides;

cystallizing the heated glycerolyzed oil by simultaneously cooling and slowly stirring for a period of about eight to seventy-two hours until a first end of crystallization temperature of between about 0.degree. and 25.degree. C. is reached; and

removing crystals from the crystallized oil at said first end of crystallization temperature.

2. The process according to claim 1, wherein said oil is a corn oil, and said first end of crystallization temperature is between 8.degree. and 10.degree. C.

3. A glycerolyzed oil produced by the process of claim 1.

4. The process according to claim 1, wherein said step of heating and maintaining is performed for one hour and said elevated temperature is 80.degree. C.

5. The process according to claim 1, wherein said step of crystallizing is performed in a container having sides using a stirrer that stirs the oil without contacting said sides and without creating vortices therein.

6. The process according to claim 1, wherein said step of removing crystals is performed by centrifuging at a temperature exceeding 0.degree. C. and not exceeding 15.degree. C. for a period of five to sixty minutes at an acceleration of 500 to 12,000 g.

7. The process according to claim 1, wherein said step of removing crystals at said first end of crystallization temperature crystals at said second end of crystallization temperature is performed by filtering at a temperature of between 0.degree. C. and 15.degree. C. through a filter cloth having an opening of 10 to 500 microns under a relative pressure of less than five bars.

8. The process according to claim 1, wherein said step of removing crystals at said first end of crystallization temperature crystals at said second end of crystallization temperature is performed by filtering at a temperature of between 0.degree. C. and 15.degree. C. through a filter cloth having an opening of 10 to 500 microns under a relative pressure of less than five bars, and by centrifuging at a temperature exceeding 0.degree. C. and not exceeding 15.degree. C. for a period of five to sixty minutes at an acceleration of 500 to 12,000 g.

9. The process according to claim 1, wherein said first end of crystallization temperature is between about 15.degree. and 25.degree. C., said step of removing crystals yields a partially decrystallized oil, the process further consisting essentially of the steps of:

heating the partially decrystallized oil until residual crystals therein are dissolved;

crystallizing the heated partially decrystallized oil by simultaneously cooling and slowly stirring for a period of about eight to seventy-two hours until a second temperature of between about 0.degree. and 15.degree. C. is reached; and

removing crystals from the cooled partially decrystallized oil at said second temperature.

10. The process according to claim 9, wherein said step of crystallizing the heated oil and said step of crystallizing the heated partially decrystallized oil are performed in a container having sides using a stirrer that stirs the oil without contacting said sides and without creating vortices therein.

11. The process according to claim 9, wherein said step of heating and maintaining is performed for one hour and said elevated temperature is 80.degree. C., and said step of heating the partially decrystallized oil is performed for one hour at 80.degree. C.

12. The process according to claim 9, wherein said step of removing crystals at said first end of crystallization temperature and said step of removing crystals at said second temperature are each performed by centrifuging at a temperature exceeding 0.degree. C. and not exceeding 15.degree. C. for a period of five to sixty minutes at an acceleration of 500 to 12,000 g.

13. The process according to claim 9, wherein said step of removing crystals at said first end of crystallization temperature and said step of removing crystals at said second temperature are each performed by filtering at a temperature of between 0.degree. C. and 15.degree. C. through a filter cloth having an opening of 10 to 500 microns under a relative pressure of less than five bars.

14. The process according to claim 9, wherein said step of removing crystals at said first end of crystallization temperature and said step of removing crystals at said second temperature are each performed by filtering at a temperature of between 0.degree. C. and 15.degree. C. through a filter cloth having an opening of 10 to 500 microns under a relative pressure of less than five bars, and centrifuging at a temperature exceeding 0.degree. C. and not exceeding 15.degree. C. for a period of five to sixty minutes at an acceleration of 500 to 12,000 g.

15. A process of preparing a fractionated glycerolyzed oil having improved crystallization stability, consisting essentially of the steps of:

heating the glycerolyzed oil and maintaining the glycerolyzed oil for one hour at 80.degree. C.;

crystallizing the heated glycerolyzed oil by simultaneously cooling and stirring the glycerolyzed oil without contacting the side of the container and without creating vortices therein for a period of about eight to seventy-two hours until a first end of crystallization temperature of between about 0.degree. and 25.degree. C. is reached, said step of crystallizing the heated glycerolyzed oil being performed without seeding the glycerolyzed oil and in an absence of alkalinizing reagents;

removing crystals from the crystallized oil by centrifuging at a temperature exceeding 0.degree. C. and not exceeding 15.degree. C. for a period of five to sixty minutes at an acceleration of 500 to 12,000 g to yield a partially decrystallized oil;

heating the partially decrystallized oil for one hour at 80.degree. C.;

crystallizing the heated partially decrystallized oil by simultaneously cooling and slowly stirring for a period of about eight to seventy-two hours until a second temperature of between about 0.degree. and 15.degree. C. is reached; and

removing crystals from the cooled partially decrystallized oil by centrifuging at a temperature exceeding 0.degree. C. and not exceeding 15.degree. C. for a period of five to sixty minutes at an acceleration of 500 to 12,000 g; whereby a fractionated glycerolyzed oil having improved crystallization stability is obtained.

16. The process according to claim 15, wherein said oil is a corn oil, and said first end of crystallization temperature is between 8.degree. and 10.degree. C.

17. The process according to claim 15, wherein said step of removing crystals from the crystallized oil and said step of removing crystals from the cooled partially decrystallized oil each further comprise the step of filtering the oil at a temperature of between 0.degree. C. and 15.degree. C. through a filter cloth having an opening of 10 to 500 microns under a relative pressure of less than five bars.

18. The process according to claim 17, wherein said oil is a corn oil, and said first end of crystallization temperature is between 8.degree. and 10.degree. C.

19. The process according to claim 16, wherein said step of removing crystals from the cooled partially decrystallized oil is performed without seeding the oil and in an absence of alkalinizing reagents.
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