Title of Invention

"A PROCESS TO ISOLATE FATTY ACID FRACTIONS, INORGANIC SALTS, GLYCEROL AND POLYGLYCEROL-RICH FRACTION FROM SWEET WATER WASTE AND THE PRODUCTS THUS OBTAINED"

Abstract A process to isolate fatty acid fractions, inorganic salts, pure gtycerol and pofyglycerol-rich fraction from sweet water waste and the end products thus obtained are disclosed. The said process comprises the steps of reacting the sweet water waste with an effective amount of acid; wherein the reaction causes an aqueous layer and fatty acid fractions to be separated and the said fatty acid fractions to be collected and the aqueous layer is retained for further reactions; neutralising the aqueous layer with an effective amount of alkali; concentrating the neutralised solution; wherein after the steps of neutralising and concentrating, a mixture of inorganic salts and crude glycerol is obtained; separating the said inorganic salts and the crude glycerol and purifying the crude glycerol into pure glycerol and polygfyeerol-rich fraction by distillation process. The end products obtained from the above-mentioned process are fatty acid fractions, inorganic salts, pure glycerol and polyglycerol-rich fraction.
Full Text A PROCESS TO ISOLATE FATTY ACID FRACTIONS, INORGANIC SALTS,
PURE GLYCEROL AND POLYGLYCEROL-RICH FRACTION FROM SWEET
WATER WASTE AND THE PRODUCTS THUS OBTAINED
FIELD OF THE INVENTION
A process to isolate fatty acid fractions, inorganic salts, pure glpcerol and polyglycerol-rich fraction from sweet water waste obtained from refining of sweet water is described. The sweet water waste undergoes acidic treatment and the fatty acid fractions are separated from the liquid. The alcohol-rich aqueous layer was then neutralised and concentrated. The insoluble inorganic salts will precipitate out of the alcohol fraction to give inorganic salts, and crude glycerol. The crude glycerol is further purified to obtain pure glycerol and polyglycerol-rich fraction.
BACKGROUND OF THE INVENTION
Oleochemical plants are continuously generating several by-products or waste, which contains useful and value-added chemicals. Sweet water wastes, yellow glycerin and glycerol residues are some of the examples of the useful by-products.
These by-products differ in their compositions, as they are dependent on the type of processes deployed by the plant, and therefore require specific treatment in order to recover the useful chemicals present in them.
There are two principal processes used to produce natural glycerol: saponification and hydrolysis of oils and/or fats. These are mainly carried out respectively in soap and fatty acid plants in the oleochemical industry. However, with the recent development of the oleochemical industry, production of methyl esters and fatty acid contribute more to glycerol supply than does the soap making.
Hydrolysis or splitting of oils and fats separates the triglycerides into the corresponding fatty acid fractions arid glycerol which is released in the form of sweet water. The sweet water generally contains about 15 to 25% glycerol. The sweet water is then subjected to multiple purification steps before the pure refined glycerol is obtained.
Sweet water waste refers to the undesirable fraction or residue generated during the refining of sweet water to produce pure glycerol. Sometimes, the sweet water waste is also known as glycerol pitch.
Sweet water waste can be very viscous, gel-like and the colour can range from brown to dark brown. It is also very alkaline and can easily absorb moisture if left exposed to air.
The sweet water waste is being continuously generated by oleochemical factories especially those involved in the manufacture of fatty acids from oil and fats. The waste generally contains crude glycerol (55 to 65%), fatty acids ( Analyses by high performance liquid chromatography and gas chromatography further indicate the presence polymeric glycerol in about 15% to 25%, such as diglycerol, trigfycerol, polyglycerol or a mixture thereof.
Polyglycerol and its corresponding esters are used as food additives, as emulsifiers, anti-spattering agent and anti-clouding in cooking and salad oil. It is also possible to use the crude glycerol containing its polymers as a feedstock for the preparation of polyurethane foams.
The wastes are usually stored in drums and taken by means of transport to a disposal site. Disposal of combustible wastes like sweet water waste has been a major a problem to the community especially in urban and densely populated areas. Burning the waste can literally means converting it into acrolein, a highly volatile compound and well known for its toxicity and very hazardous to life. Attempts have been made to isolate useful components from these oleochemical wastes including sweet water waste.
With the prosperity of the oleochemical industry and with current awareness of environmental issues among consumers, there is a strong need to deploy the concept or recycle and recover.
SUMMARY OF THE INVENTION
It is therefore the objea of the present invention to provide a process to isolate fatty acid fractions, inorganic salts, pure glycerol and polyglycerol-rich fraction from sweet water wastes.
It is still another objea of the present invention to provide a process, which is simple and also cost-effective and yet efficiently reduces the wastage of sweet water.
It is still another objea of the present invention to reduce the environmental problems caused by sweet water waste.
These and other objects of the present invention are accomplished by providing a process to isolate fatty acid fractions, inorganic salts, pure glycerol and polyglycerol-rich fraction from sweet water waste.
The invention consists of certain novel features and a combination of parts hereinafter fully described and illustrated in the accompanying drawings, and particularly pointed out in the appended claims, it being understood that various changes in the details may be without departing from the scope of the invention, or sacrificing any of the advantage of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
For the purpose of facilitating an understanding of the invention, there is illustrated in the accompanying drawings a preferred embodiment thereof, from an inspection of which, when considered in connection with the following description, the invention, its construction and operation, and many of its advantages should be readily understood and appreciated.
Figure 1 is the flow chart to illustrate the steps of producing sweet water waste from sweet water.
Figure 2 is the flow chart to demonstrate the steps of producing fatty acid fractions, inorganic salts, pure glycerol and polyglycerol-rich fraction from sweet water waste according to the preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
In the present invention, sweet water waste is subjected to extraction procedure, using common reagents and chemicals, which separates the sweet water waste into four major components such as fatty acid fractions, inorganic salts, crude glycerol and polyglycerol-rich fraction as shown in Table 1.
The inorganic salts present in sweet water waste can be precipitated out with or without the presence of organic solvents. The said organic solvent functions as a catalyst to reduce the time taken to precipitate the inorganic salt The organic solvent is selected from a group consisting of any short-chained alcohols, preferably MeOH.
The fatty acid fractions were analysed by gas chromatography without further purification. The fatty acid fractions' compositions are as demonstrated in Table 3, where the compositions can vary from one sample to another.
In this isolation process, sweet water waste was treated with acid to pH less than 7 and the free fatty acid fractions can be separated from the aqueous layer. Any kinds of mineral acids and organic acids can be used in this process. In the preferred embodiment of the present invention, the mineral acids include HNO3, H2SO4 and HC1, preferably H2SO4
The aqueous layer was then neutralised by adding alkali, wherein the said alkali is selected but not confined to NaOH and KOH, preferably NaOH and concentrated to give glycerol-rich liquid and inorganic salts by removing the water from the solution. The water may be
removed by evaporation from the solution by any means of an evaporator such as a rotary evaporator. The solution is now called as the trialcohol fraction or crude glycerol fraction which is a mixture of glycerol and polyglycerol.
The inorganic salts will precipitate out of the said crude glycerol fraction. Both products could then be separated.
The crude glycerol isolated could then be further refined to pure glycerol 98.5 to 99.8% purity. A pure and refined glycerol is usually attained by high vacuum distillation as exemplified in Table 2. However, it has to be noted that any other kinds of distillation procedures can also be used for this purpose and is within the knowledge of a person having an ordinary skill in the art.
It is also a common practise in the oleochemical industry that to further purify the distilled glycerol via any other methods such as passing h through ion exchange resins or activated carbon columns or any other suitable methods.
The identification of pure glycerol may be carried out via spectrometric methods such as FTlR, 1H NMR or the following standard methods usually practised in oleochemical plants such as glycerol content, moisture content, ash contents, acidity, gas chromatography and refractive index.
As the result of this purification step, pure glycerol with the purity of 98.5 to 99.8 is obtained together with polyglycerol-rich fraction.
The temperature condition is not critical to the invention. It is normally carried out at room temperature or at an elevated temperature less than 60°C. However, the preferred temperature is at room temperature. Thus, the processes can still be run efficiently without jeopardising the quality of the processes and the end products even at different temperatures.
Table 1: Composition of Sweet Water Waste (%)
(Table Removed)
composition varies with samples
Table 2: Some of the Characteristics of the Isolated Glycerol Obtained from Sweet Water Waste
(Table Removed)
*Pure glycerol was obtained from the crude glycerol isolated from sweet water waste via small-scale vacuum distillation.
Table 3: Fatty Acids Profiles of the Fatty Acid Fractions Isolated from Sweet Water Waste
(Table Removed)
The composition varies with samples
EXAMPLES
Example 1
1kg of sweet water waste was stirred in 500 ml of H2O and then treated with concentrated H2SO4 at room temperature to the desired pH (less than 7). The freed fatty acid fractions layer was separated from the liquid followed by neutralisation of the aqueous later with NaOH. Rotary evaporator is used to concentrate the aqueous layer. The resulting inorganic salts that settled at the bottom of the fraction was separated and isolated. The crude glycerol obtained was further refined by high vacuum distillation. The polyglycerol-rich fraction is then obtained from the residue.
Example 2
1kg of sweet water waste was stirred in 500 ml of H2O then treated with concentrated H2SO4 as illustrated in Example 1. The freed fatty acid fractions layers were then concentrated followed by an addition of MeOH to the concentrated organic fraction. The mixture was allowed to stand at room temperature. The inorganic salts that precipitated out from the methanolic fraction could be then separated and isolated. The solvent was removed to give crude glycerol which can be further refined by vacuum distillation. The polyglycerol-rich fraction is then obtained from the residue.
Example 3
The crude glycerol obtained from Examples 1 and 2 was subjected to a high vacuum distillarion where pure glycerol could be obtained The pure glycerol was about 98.5 to 99.8% purity. The polygtycerol-rich fraction is then obtained from the residue.





CLAIMS
1. A process to isolate fatty acid fractions, inorganic salts, pure glycerol and polygrycerol-
rich fraction from sweet water waste, wherein the said process comprises the steps of:
a) reacting the sweet water waste with an effective amount of acid; wherein the reaction
causes an aqueous layer and fatty acid fractions to be separated and the said fatty acid
fractions to be collected and the aqueous layer is retained for further reactions;
b) neutralising the aqueous layer with an effective amount of alkali;
c) concentrating the neutralised solution; wherein after the steps of neutralising and
concentrating, a mixture of inorganic salts and crude glycerol is obtained;
d) separating the said inorganic salts and the crude glycerol; and
e) purifying the said crude glycerol to obtain pure glycerol and polyglycerol-rich fraction
by distillation process.

2. A process as claimed in claim 1, wherein the acid is selected from the group consisting of
mineral or organic acids, preferably mineral acids.
3. A process as claimed in claim 2, wherein the acid is selected from the group consisting of
HNO3, H2SO4 and HC1, preferably H2SO4.
4. A process as claimed in claim 1, wherein the alkali is NaOH and KOH, preferably
NaOH
5. A process as claimed in claim 1, wherein the process is conducted at temperature less
than 60°C, preferably at room temperature.
6. A process as claimed in claim 1, wherein organic solvent is optionally added to further
precipitate the inorganic salt and functions as a catalyst.
7. A process as claimed in claim 6, wherein the organic solvent is selected from a group of
any short-chained alcohols, preferably MeOH.
8. Products obtained from a process to isolate fatty acid fractions, inorganic salts, pure
glycerol and polyglycerol-rich fraction from sweet water waste, wherein the said process
comprises the steps of:

a) reacting the sweet water waste with an effective amount of acid; wherein the reaction
causes an aqueous layer and fatty acid fractions to be separated and the said fatty acid
fractions to be collected and the aqueous layer is retained for further reactions;
b) neutralising the aqueous layer with an effective amount of alkali;
c) concentrating the neutralised solution; wherein after the steps of neutralising and
concentrating, a mixture of inorganic salts and crude glycerol is obtained;
d) separating the said inorganic salts and the crude glycerol; and
e) purifying the said crude glycerol to obtain pure glycerol and polyglycerol-rich fraction
by distillation process.
wherein the products obtained are fatty acid fractions, inorganic salts, pure glycerol and polyglycerol-rich fraction.
9. Products as claimed in claim 8, wherein the acid is selected from the group consisting of
mineral or organic acids, preferably mineral acids.
10. Produas as claimed in claim 9, wherein the acid is selected from the group consisting of
HNO3, H2SO4 and HCl, preferably H2SO4.
11. Produas as claimed in claim 8, wherein the alkali is seleaed from the group consisting of
NaOH and KOH, preferably NaOR
12. Produas as claimed in claim 8, wherein the process is conducted at temperature less than
60°C, preferably at room temperature.
13. A process as claimed in claim 8, wherein organic solvent is optionally added to further
precipitate the inorganic salt and functions as a catalyst
14. A process as claimed in claim 13, wherein the organic solvent is selected from a group of
any short-chained alcohols preferably MeOH.
15. A process to isolate fatty acid fractions, inorganic salts, pure
glycerol and polyglycerol-rich fraction from sweat water waste
substantially as herein described with reference to foregoing
examples and as illustrated by the accompanying drawings.
16. Product obtained from a process isolate fatty acid fractions,
inorganic salts, pure glycerol and polyglycerol-rich fraction from
sweat water waste substantially as herein described with
reference to foregoing examples and as illustrated by the
accompanying drawings.

Documents:

636-del-2002-abstract.pdf

636-del-2002-claims.pdf

636-del-2002-correspondence-others.pdf

636-del-2002-correspondence-po.pdf

636-del-2002-description (complete).pdf

636-del-2002-drawings.pdf

636-del-2002-form-1.pdf

636-del-2002-form-18.pdf

636-del-2002-form-2.pdf

636-del-2002-form-3.pdf

636-del-2002-form-4.pdf

636-del-2002-form-5.pdf

636-del-2002-gpa.pdf

636-del-2002-pa.pdf

636-del-2002-petition-138.pdf

abstract.jpg


Patent Number 220519
Indian Patent Application Number 636/DEL/2002
PG Journal Number 31/2008
Publication Date 01-Aug-2008
Grant Date 29-May-2008
Date of Filing 13-Jun-2002
Name of Patentee MALAYSIAN PALM OIL BOARD,
Applicant Address 6,PERSIARAN INSTITUSI, BANDAR BARU BANGI, 43000 KAJANG, SELANGOR, MALAYSIA.
Inventors:
# Inventor's Name Inventor's Address
1 DR. HASSAN HAZIMAH ABU
2 DR. AHMAD SALMIAH
3 DR. LYE OOI TIAN
PCT International Classification Number C02F 1/52
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 PI20013757 2001-08-10 Malaysia