Enzymatic degumming

Abstract

The present invention relates to a method for treating vegetable oils and/or animal fats. The method comprises adjusting temperature, treatment with acid, adjusting pH, contacting the aqueous mixture with enzyme, crystallization of high melting glycerides and separation.

Claims

1. A method for treating vegetable oils and/or animal fats, comprising the following steps: (i) adjusting the vegetable oils and/or animal fats to a temperature within a range from about 20 to about 90 C.; (ii) pre-treating the vegetable oils and/or animal fats with acid for at least 1 minute; (iii) adjusting a pH of the pretreated vegetable oils and/or animals fats with lye to a pH within a range from about 4 to about 8 at a temperature of at least 20 C. to obtain an aqueous mixture; (iv) adding enzymes to the aqueous mixture to form lysophospholipids and free fatty acids from phospholipids in the aqueous mixture; (v) reducing a temperature of the aqueous mixture comprising the lysophospholipids and the free fatty acids obtained in step (iv) to a crystallization temperature of high melting glycerides and conducting centrifugation; (vi) separating the aqueous mixture into an aqueous phase and a treated phase comprising treated vegetable oils and/or treated animal fats; and (vii) optionally treating the treated phase with hot water or with silica adsorption.

2. The method according to claim 1, wherein the temperature in step (i) is adjusted within a range from about 40 to about 90 C.

3. The method according to claim 1, wherein in the pre-treating step (ii) the vegetable oils and/or animal fats is treated with acid from about 1 to about 60 minutes.

4. The method according to claim 1, wherein the pH in step (iii) is adjusted with the lye to a pH within a range from about 4 to about 8 at a temperature from about 40 to about 60 C.

5. The method according to claim 1, wherein the temperature of the aqueous mixture in step (v) is adjusted by a cooling rate and by a residence time to optimize crystallisation.

6. The method according to claim 1, wherein a temperature of the aqueous mixture in separation step (vi) is adjusted to facilitate separation.

7. The method according to claim 6, wherein the temperature of the aqueous mixture in separation step (vi) is adjusted to within the range of from about 15 to about 50 C.

8. The method according to claim 1, wherein the enzyme in treatment step (iv) is a phospholipase enzyme.

9. The method according to claim 1, wherein the acid in step (ii) is selected from the group consisting of phosphoric acid, acetic acid, citric acid, tartaric acid, succinic acid, and a combination thereof.

10. The method according to claim 1, wherein the temperature in step (i) is adjusted to be within the range from about 60 to about 90 C.

11. The method according to claim 1, wherein the mixing of enzyme in step (iv) is continued within the range from about 1 min to about 6 hours.

12. The method according to claim 1, wherein the mixing of the lye in step (iii) is continued within the range from about 1 min to about 4 hours.

13. The method according to claim 1, wherein the lye in step (iii) is selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium silicate, sodium carbonate, calcium carbonate, and a combination thereof.

14. The method according to claim 1, wherein in the pre-treating step (ii) the vegetable oils and/or animal fats is treated with acid from about 5 to about 60 minutes.

15. The method according to claim 1, wherein in the pre-treating step (ii) the vegetable oils and/or animal fats is treated with acid from about 20 to about 40 minutes.

16. The method according to claim 1, wherein the temperature of the aqueous mixture in step (v) is adjusted by a cooling rate within a range of from about 0.5 C. per hour to about 5 C. per hour, and a residence time within a range of from about 4 to 24 hours.

17. The method according to claim 1, wherein the temperature of the aqueous mixture in step (v) is adjusted by a cooling rate within a range of from about 0.5 C. per hour to about 5 C. per hour, and a residence time within a range of from 6 to 12 hours.

18. The method according to claim 1, wherein the enzyme in treatment step (iv) is selected from the group consisting of a phospholipase A enzyme, a phospholipase C enzyme, and combinations thereof.

19. The method according to claim 1, wherein the acid in step (ii) is selected from the group consisting of phosphoric acid and citric acid and combinations thereof.

20. The method according to claim 1, wherein the lye in step (iii) is selected from the group consisting of sodium hydroxide, potassium hydroxide and combinations thereof.

21. The method according to claim 1, wherein the enzymes comprise phospholipase A, and phospholipase C is not present.

Description

EXAMPLE 1

(1) The equipment used in this experiment was an oil bath, Erlenmeyer flasks 500 ml, magnetic stirrer with heating and temperature control, an Ultra Turrax, a laboratory centrifuge. FFA is analyzed according to method according to American Oil Chemists' Society, AOCS, Ca 5a-40, moisture is analyzed according to method AOCS Ca 2b-38, and phosphorus is analyzed according to method DIN EN 14107.

(2) Materials used were:

(3) 1. Citric acid, monohydrate

(4) 2. Sodium Hydroxide, dry

(5) 3. Enzyme, Lecitase Ultra, i.e. a phospholipase A enzyme.

(6) 4. Water

(7) The crude sunflower seed oil was heated in oven to 70 C. to ensure all the wax crystals are melted and dissolved in the oil. Two 500 ml. Erlenmeyer flasks, A and B, were used, one for normal enzymatic deep degumming (A) and the other for cold enzymatic deep degumming (B). To each Erlenmeyer flasks were 250 g of oil were added, and the flasks were placed in a 55 C. oil bath. The oil was stirred with a magnetic rod during the whole reaction, i.e. approx. 350 rpm.

(8) A citric acid solution, i.e. 5 ml, was prepared by dissolving 1.78 g citric acid monohydrate in distilled water. A sodium hydroxide solution was prepared, i.e. 5 ml, by dissolving 0.5075 g sodium hydroxide pellets in distilled water.

(9) To each flask were 0.5 ml of citric acid solution added, and the mixture were mixed by using an Ultra Turrax at high speed, approx. 24000 rpm, for min. After 1 hour 0.5 ml of NaOH solution were added and the mixtures were mixed with an Ultra Turrax for min. To each flask were 0.012 ml of enzyme added together with water summing up to a total of 6 ml for each sample, and the mixing continued for additional min.

(10) After 3 hours of enzyme treatment, the oil bath for flask A is heated to 80 C. to inactivate the enzyme; while flask B was moved together with the magnetic agitator to fridge (7-8 C.), and the agitation was kept at ca. 40 rpm for an overnight.

(11) After hour heating at 80 C., the oil from flask A for 5 min was centrifuged at 2000g. The moisture, FFA and phosphorus content in the light phase (oil phase) were analysed.

(12) After an overnight agitation in the fridge, flask B and the magnetic agitator were removed from the fridge, and the agitation was kept at room temperature (about 22 C.) for ca. 15 min. The oil from flask B was centrifuged for 5 min. at 2000g and the moisture, FFA and phosphorus content in the light phase were analysed.

(13) The residual phosphorus content in the degummed oil is about 1 ppm only, which implies the degumming in both samples is complete.

(14) TABLE-US-00001 TABLE Analysis Crude oil Sample A Sample B Acid value 0.84 0.85 0.82 [mg KOH/g] Moisture 947 1342 669 [mg/kg] Phosphorous 265 0.9 1.1 [mg/kg]

(15) On the other hand, it was found some wax was removed together with the gum from the oil in the cold enzymatic deep degumming (B) sample after centrifuge separation. However, the amount of wax was not analyzed in this experiment.

(16) Conclusion: The sunflower seed oil is successfully degummed in the cold enzymatic degumming process. Even though the separation temperature is much lower than that in ordinary degumming process, the residual phosphorus content in cold enzymatic degummed oil is at the same level as in the ordinary degummed oil.

EXAMPLE 2

(17) The process according Example 1 is repeated on another batch of sunflower oil which is a mixture of crude sunflower oil and water degummed sunflower oil. It contains 177 ppm phosphorus and min. 1000 ppm wax. The result of the two samplesnormal enzymatic deep degumming (A) and the other for cold enzymatic deep degumming (B) is summarized in the table below.

(18) TABLE-US-00002 TABLE 2 Analysis Crude oil Sample A Sample B Acid value 2.10 2.19 2.21 [mg KOH/g] Phosphorous 177 8 10 [mg/kg] Wax 1000* 1000* 152 [mg/kg] *The instrument can only analyze the wax content up to 1000 ppm.

(19) Conclusion: The sunflower oil is successfully degummed and dewaxed in the cold enzymatic degumming process. The residual wax in degummed oil is less than 15% of feed oil.