Organic compounds -- part of the class 532-570 series – Organic compounds – Fatty compounds having an acid moiety which contains the...
Reexamination Certificate
2001-05-31
2003-11-18
Carr, Deborah D. (Department: 1621)
Organic compounds -- part of the class 532-570 series
Organic compounds
Fatty compounds having an acid moiety which contains the...
C554S206000, C435S067000
Reexamination Certificate
active
06649781
ABSTRACT:
RELATED APPLICATIONS
This application claims priority under 35 U.S.C. §119 from Malaysian patent application serial number PI 20005886, filed Dec. 14, 2000.
TECHNICAL FIELD OF THE INVENTION
This invention relates to a process for the recovery of minor components and refining of vegetable oils and fats from crude vegetable oils and fats, in particular, a process for the recovery of minor components and refining of vegetable oils and fats from seed oil, pulp oil and other vegetable matter.
BACKGROUND OF THE INVENTION
Crude palm oil contains less than 5% of free fatty acid (FFA). The main fatty acids are palmitic acid and oleic acid. During fractionation, fatty acid is slightly concentrated in the palm olein. Crude palm oil contains 600-1000 ppm of tocotrienol/tocopherol mixture. The tocotrienol presence in palm oil are &ggr;-tocotrienol, &agr;-tocopherol, &agr;-tocotrienol and &dgr;-tocotrienol in an approximate ratio of 5:2:2:1. Tocotrienol is also enriched in the palm olein during fractionation. Tocotrienol was claimed to be very effective in cholesterol lowering, preventing arteriosclerosis and stroke, inhibits breast cancer cells, protecting the skin against the effects of ultraviolet radiation and as powerful antioxidant.
Typical crude palm oil contains more than 4% of diglyceride. Diglyceride is considered undesirable as it affects crystallization during fractionation. Based on long term human study on feeding of diglycerides-rich cooking oil, diglyceride was said to be able to reduce serum triglycerides, increased serum high density lipoprotein (HDL)-cholesterol and reduction in plasminogen activator inhibitor.
Crude palm oil contains about 500-700 ppm of carotene. The main carotene components are &bgr;-carotene and &agr;-carotene. During fractionation, carotene is concentrated in the olein (liquid) fraction. Crude palm olein can contain up to 1500 ppm of carotene whereas crude palm stearin (the solid fraction) has much lower carotene (as low as less than 200 ppm). Consumption of a mixture of natural carotene was claimed to provide protection towards free radical mediated degenerative diseases such as cancer and cardiovascular diseases. It was also claimed that &agr;-carotene but not &bgr;-carotene inhibited liver carcinogenesis. It was also claimed that intake of palm carotene inhibits skin peroxidation induced by ultraviolet radiation.
There are patents describing the production of refined red palm oil from crude palm oil. These include U.S. Pat. No. 5,932,261 and Australian Patent Application No. P18770/88. All these patents involved molecular distillation of palm oil at relatively high temperature to remove the fatty acid.
There are also patents describing the production of carotene concentrate from crude palm oil. These include U.S. Pat. Nos. 5,157,132, 6,072,092, 5,019,668 and U.K Patent No. GB2160874A, GB2218989A and GB1515238. Again all these patents involved pretreatment to the free fatty acid, molecular distillation and followed by the process of post treatment such as using adsorbents.
This invention relates to the process of producing refined red oils and fats, carotene concentrate, distilled fatty acid, tocotrienol and sterol concentrate, and diglyceride from carotene-containing natural oils and fats and has particular but not exclusive application to the process of producing these products from crude palm oil and its fractionated products by first removing the polar components prior to transesterification and therefore no post-treatment is necessary after distillation.
This invention has many advantages. It can refine palm oil and palm oil fractionated products without destroying the carotene at a lower vacuum distillation temperature since the polar components including that of odoriferous materials and free fatty acid are removed by alcohol extraction prior to distillation. It also can refine crude palm oil or its fractions into the refined, bleached and deodorized (R.B.D) oils without using degumming agent such as phosphoric acid and deodorized at a significantly lower temperature as most of the free fatty acid and odoriferous materials have been removed.
This invention also enables transesterification to be carried out without pre-esterification of free fatty acid. It also enables production of carotene concentrate without the need of post-distillation treatment such as using adsorbent. As the polar components had been removed from the oil prior to transesterification, the transesterification reaction was carried out without interference from the unsaponifiable matter and carotene remained in the residue. The processes described in the present invention are simpler and cost-effective as compared to that described in other patents on carotene recovery from palm oil. This invention also enables the recovery of FFA, tocotrienol, tocopherol, sterol and diglyceride and other useful minor components of palm oil.
SUMMARY OF THE INVENTION
The object of the present invention is to provide a process for the recovery of minor components and refining of vegetable oils and fats from crude vegetable oils and fats without destroying naturally occurring components in the crude vegetable oils and fats.
Accordingly, there is provided a process for the recovery of minor components and refining of vegetable oils and fats wherein said process is:
A process for the recovery of minor components and refining of vegetable oils and fats without destroying naturally occurring components, said process comprising the steps of:
a) removal of polar components from the crude vegetable oils and fats using lower alkyl alcohol or any lower alkyl alcohol-water mixture;
b) removal of alcohol from the product obtained in step (a) by distillation;
c) addition of suitable quantity of bleaching earth to the product obtained in step (b) at normal bleaching temperature followed by filtration; and
d) deodourization of the product obtained in step (c) at a low temperature.
This invention will be clearly understood and apparent with reference to the detailed description which follows.
DETAILED DESCRIPTION OF THE INVENTION
The features and details of the invention, either as steps of the invention or as combinations of parts of the invention will now be described. It will be understood that the particular embodiments of the invention are shown by way of illustration and not as limitations of the invention. The principle features of the invention may be employed in various embodiments without departing from the scope of the invention.
Carotene is non-polar in nature. It is freely soluble in oils and fats. Its solubility in lower alkyl alcohol is low. Natural oils and fats consist mainly of triglyceride, which also has low solubility in lower alkyl alcohol such as methanol and ethanol. Oils and fats are soluble in n-propanol, isopropanol and other lower alkyl alcohol. Addition of water or a mixture of these lower alcohol water mixtures can be used to form two phases in the presence of oils and fats.
By using polar solvent such as lower alkyl alcohol or lower alkyl alcohol-water mixture, the polar components such as FFA, tocopherol, tocotrienol, sterol, triterpene alcohol, mono-glyceride, di-glyceride, glycolipid and phospholipid can be extracted out from oils and fats, remaining the non-polar components such as carotene, squalene and triglyceride.
The oil or fat after lower alkyl alcohol extraction can be subjected to washing with water. Residual solvent and/or water can be vacuum distilled at a temperature less than 100° C. without destroying tocopherol and tocotrienol in the methanol extract. The mixture of FFA, tocopherol, tocotrienol, sterol, triterpene alcohol, mono-glyceride and di-glyceride can be used for their recovery.
A 1-liter crude palm olein of sample was vigorously stirred with methanol at oil to methanol ratios of 1:1, 1:2, 1:3 and 1:4. Table 1 summarizes the results
Weight of
Oil: MeOH
Carotene,
MeOH
ratio
Extraction stages
FFA, %
ppm
extract, g
Initial
4.30
873
1:1
After 1
st
extraction
2.56
870
25.3
1:1
After 2
nd
extraction
1.67
875
18.5
1:1
After 3
rd
extraction
0.98
873
14.8
1
Carr Deborah D.
Palm Specialty Products, SDN. BHD.
Wolf Greenfield & Sacks P.C.
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