Organic compounds -- part of the class 532-570 series – Organic compounds – Fatty compounds having an acid moiety which contains the...
Reexamination Certificate
1998-03-31
2002-11-26
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...
C554S008000, C554S020000, C554S021000, C554S191000, C554S210000
Reexamination Certificate
active
06486335
ABSTRACT:
This invention relates to a process for the preparation of refined hard sugarcane wax having improved qualities from press mud
Sugarcane wax (the hard variety) is a replacement of the commonly used carnauba wax. By nature sugarcane wax (the hard variety) is a type of microcrystalline wax having a high potential used in preparation of several important industrial products. Its potential use is wide in industry. The refined variety of the hard sugarcane wax having its potential use in: (a) Medicines, (b) in sweet meats and pastries, (c) in tinned food products, (d) in castings and recordings, (e) in carbon papers, (f) in preparation of carbonless carbon papers, (g) in electrical insulation of cables and wires, (h) in preparation of various types of paints, varnishes and polishes including shoe polishes, car polishes and floor polishes, (i) in preparation of coloured pencils, crayons, water and oil paints, (j) in cosmetics, (k) in preparation of emulsion paints for spraying. In fact, it has its most likely entries into all the branches of industries where carnauba wax is mostly used. In bulk also it can be produced many times more than any other plant waxes combined together. The raw material, press mud is a rejected waste material of sugarcane industries, that causes the unwanted problem of pollution to the surrounding supurbs of the sugar mills on accumulation. Also, the availability of the press mud is no problem at all throughout the year. While carnauba plant is a seasonal plant that produces extractable waxes only in marked period of a year.
(ii) The CHEMISTRY and TECHNOLOGY of WAXES by ALBIN H. WARTH Wax Research Consultant, Formerly Chemical Director The Crawn Cork and Seal Company Baltimore, Md.
REINHOLD PUBLISHING CORPORATION New York CHAPMAN & HALL LTD., LONDON.
The mode and the process of refining sugarcane wax (the hard variety) as mentioned above probably implies high acid values and saponification numbers to the presently available refined hard sugarcane wax of the world market.
The value of the wax increases with its colour and refining techniques. In the known process isolation of sugarcane wax from press mud (sugarcane press mud) is done commercially by use of solvents such as benzene, toluene, heptane and sometimes turpentine oils. The production of sugarcane wax is mainly been done only in one or two places in the world commercially. In India, Ravalgaon Sugar Industry prepares some amount of cane wax for its own use. The refining of the crude cane wax has been done by these industries by methods described in brief on the previous page.
The main object of the present invention is to develop a process for isolation and refining crude sugarcane-wax by using polar solvent such as carbon tetrachloride (CCl
4
) and activated charcoal. Another object of this invention is to provide a process which can produce hard wax having low acid values and low saponification number. Still another object of this invention is to produce simultaneously soft wax, pitch and starting material for agro manures as by-product.
The use of activated charcoal in refining crude sugarcane wax has not yet been included in industries producing sugarcane wax from press mud wastes. This is so because it is considered to be a mild agent for performing refining of sugarcane wax. Stronger refining agents such as sulphuric acid, nitric acid and chromic acids are presently being used for refining sugarcane wax in industry. Further refining of the industrial sugarcane wax is being done by the use of low pressure vacuum distillations. Probably, by the use of such methods (acid treatment) may be the cause of imparting higher acid values and higher saponification numbers to the presently available limited quantities of hard sugarcane wax of the world market.
Accordingly, the present invention provides a process for the preparation of refined hard sugarcane wax having improved qualities from press mud which comprises
(1) digesting press mud with a non polar solvent such as carbon tetrachloride (CCl
4
), benzene (C
6
H
6
) or toluene (C
7
H
8
) in presence of activated charcoal, where in the ratio of the non polar solvent:activated charcoal:press mud ranges from 3 liters to 1.50 liters:50 gm to 20 gm:1 kg to 500 gm (60 to 75:1:20 to 25);
(2) separating the residue by known methods;
(3) removing the solvent by conventional methods followed by treating the crude sugarcane wax obtained with hot isopropyl alcohol to get the wax in solution and pitch as residue;
(4) separating the said wax in solution by known methods and cooling to room temperture so as to get the said wax precipitated;
(5) washing thoroughly with water till the isopropyl alcohol is removed and drying to get the hard sugarcane wax;
(6) if desired recycling the isopropyl alcohol (I.P.A.) to step (3) and then treating the said sugarcane wax with hot water for further refining.
The present invention provides a better process than the existing commercial method of isolation and refining of sugarcane hard wax having low acid values and saponification numbers from press mud waste. In the process of the present invention carbon tetrachloride (CCl
4
) has been used as solvent for extraction of press mud in isolating sugarcane wax. This solvent has not yet been used industrially for extraction of sugarcane wax from press mud. In the extraction of press mud by the method of the present invention, carbon tetrachloride has been found as efficient as any other polar solvents used industrially for the purpose. Moreover, CCl
4
have its advantages also. It is non-carcenogenic and non-imflamable. Activated charcoal is used for refining the crude cane wax. The product, sugarcane wax obtained by this process has a nominal acid value and saponification number. The colour of the hard wax obtained is light cream in colour, which is being highly preferred in the present world market. This is being made clear in the Table 1. The product by the process of the present invention is being compared with that of the commercial product present in the American market.
TABLE 1
HARD SUGARCANE WAX FROM
Present Process
American market
Chemical
Double
Double
characteristic
Refined
refined
Refined
refined
determined
product
product
product
product
1.
Colour
Light yellow
Light
Light
Dull
(Cream)
cream
brown
yellow
2.
Melting
72° C. to
80° C. to
78°
77° C. to
point ° C.
75° C.
82° C.
82° C.
3.
Specific
0.975 to
0.955 to
0.991 to
0.961 to
gravity
0.978
0.961
0.999
0.970
4.
Acid value
6.64
3.78
13
8 to 23
5.
Saponifica-
6.894
2.90
57
55 to 95
tion number
A reference can be made to page number 228 of THE CHEMISTRY AND TECHNOLOGY OF WAXES BY ALBIN h. WARTH.
This process of the present invention is a successfully developed method of acquiring high grade refined sugarcane wax (the hard variety) by using CCl
4
for extraction of press mud and activated charcoal for refining the wax extracted. The use of mineral acids and distillation at reduced pressure employed in the hitherto known process for refining the crude wax and the hard wax obtained has been successfully avoided. For further refining, the wax obtained was treated and melted in hot water and then cooled to room temperature to recover the wax. This process removes any water soluble impurities if present, from the wax. This product prepared by the present invention has a nominal acid value and saponification number, and, in appearance, the wax is creamy-coloured lumps.
According to the present process, the air-dried press mud was digested with a nonpolar organic solvent, such as carbon tetrachloride (CCl
4
), benzene (C
6
H
6
) and toluene (C
4
6
6
) in the ratio of 2:3 to 2:5 at a temperature range of 80° C. to 90° C. (for CCl
4
and benzene) and up to 110° C. for tolouene. The digestion of the press mud has been done with any of these solvents for about 3 (three) to 7 (seven) hours at a stretch in presence of activated charcoal. The digested lot has been cooled to room temperature and filtered under subjection to vacuum filtration system by the use of an exhaust pump The residues on the filter pad washed three to fou
Carr Deborah D.
Council of Scientific & Industrial Research (CSIR)
Dinesh Agarwal, P.C.
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