Sugar – starch – and carbohydrates – Products – Miscellaneous
Reexamination Certificate
2001-03-28
2002-09-10
Brunsman, David (Department: 1755)
Sugar, starch, and carbohydrates
Products
Miscellaneous
C127S034000, C536S002000
Reexamination Certificate
active
06447614
ABSTRACT:
The invention is related to an improved method for the preparation of organic materials, such as pectin, from sugar beet pulp, from which sugar has been extracted. In accordance with the invention, said sugar beet pulp, from which sugar has been extracted, is pre-treated in a biotechnical process in mildly acidic, deoxidizing conditions prior to hydrolysis or extraction of the desired products. In the biotechnical process the fresh pulp is subjected a deoxidizing, mildly acidic pre-treatment, and the pulp is allowed to stabilize in substantially oxygen-free conditions. The stabilized pulp, which is stable for months in air-tight storage, is used as a raw material in the preparation of sugar beet pectin and related products, such as araban, arabinose, galactan and ferulic acids.
DESCRIPTION OF THE PRIOR ART
Sugar beet hemicellulose is a complex hydrocolloid based on galacturonic acid polymers, the backbone polymer chain comprising regions composed of rhamnose and galacturonic acid for connecting polygalacturonic acid units. Araban and galactan polymer chains are connected to the rhamnose units in these hairy regions.
A galacturonic acid chain is partly acetylated and methylated. Xylose and ferulic acid units are present in the side chains. Pectin can be extracted from sugar beet pulp after mild acid hydrolysis. The composition of pectin depends on the extraction conditions. Some pectic substances, such as arabans, can be alternatively extracted after alkaline hydrolysis. In his patent (U.S. Pat. No. 5,008,254), Michael Weibel describes processes for carrying out the hydrolysis in acid conditions (pH below 4.5) or in alkaline conditions (pH over 9.0) at elevated temperatures.
WO 97/30215 (Wong, E., et al.) discloses use of fermented sugar beet pulp for making paper or cardboard. The preparation of pectin and related compounds is not disclosed.
A conventional process for the preparation of sugar beet pectin is by acid hydrolysis at a pH of about 1.5, followed by neutralization, purification by filtration and precipitation of the pectins with alcohol. McCleary et al. disclose an improved method of preparing araban from fresh sugar beet pulp by extraction with an alkaline lime solution (U.S. Pat. No. 5,250,306). Schiweck et al. prepared L-arabinose from sugar beet araban or beet pulp by hydrolysis in alkaline conditions (U.S. Pat. No. 4,816,078).
The raw material for pectins has been either fresh or dried pulp. Fresh pulp is available only for a short period during the sugar beet season. Consequently, dried pulp has usually been employed.
ADVANTAGES OF THE INVENTION
The use of fresh pulp in the preparation of pectins is not economically feasible due to its limited availability. On the other hand, when the pulp is dried, reactions occur causing colour formation, lower quality of the products obtained from the pulp, and reduced pectin yield. In practice no suitable raw material for sugar beet pectin has been found, and consequently the production and use of this excellent plant hydrocolloid has remained very low.
It has now been discovered that the use of non-dried sugar beet pulp, from which sugar has been removed and which has been subjected to biotechnical pre-treatment in acidic, deoxidizing conditions, results in an improvement in the total process increasing the yields of the desired products from the raw material, which remains stable in storage and is available throughout the year. In the pre-treatment the free sugars still present in said pulp, from which sugar has been removed, are oxidized into organic acids and oxygen is removed, but the pectic substances are not affected. Kept away from light in tight storage, i.e. in substantially oxygen-free conditions, the treated pulp remains stable for months. This stable pulp is an excellent raw material in the preparation of sugar beet pectin and related compounds, such as araban, galactan, L-arabinose, ferulic acids, L-rhamnose, etc.
DESCRIPTION OF THE INVENTION
Fresh, pressed sugar beet pulp, from which sugar has been extracted and whose dry substance content is about 20 to 25 percent by weight, is pre-treated by reducing its pH to about 4, preferably by mixing the pulp with a suitable acid solution. Organic acids, such as formic acid, lactic acid, acetic acid and/or mixtures thereof are effective and easy to use. Commercially available acid mixtures include e.g. “Ensimax”, which consists of formic acid and lignosulphonate, and silage (AIV) acid consisting mainly of formic acid. The choice of acid depends on the price and pre-treatment conditions. Very volatile acids, such as formic acid, can cause irritation if used without proper protection. The lime content of the pressed pulp is preferably low, i.e. no lime or aluminium is added to the beet pulp (the cossette) to facilitate the pressing at the final stage of the sugar (saccharose) separation process. After the pressing the temperature of the pulp is about 60° C. and pre-treatment is carried out preferably immediately after the pressing before the pulp cools off.
The pre-treated pulp having a pH of about 4 is preferably packaged in air-tight storage and allowed to stabilize. The tight storage can be e.g. a plastic bag or tube made of polyethene, or what is known as a flat silo. The protection prevents light and air (oxygen) from accessing the treated pulp. The enzyme activity of lactic acid bacteria present in the fresh pulp causes oxidation of free sugars during the stabilization. Organic acids, mainly lactic acid, are formed. The deoxidizing reaction with acid formation as a result removes oxygen and free sugars from the material and prevents further fermentation of the pulp. The obtained pulp, preferably having a pH of 3.5 to 4.5 (most preferably 3.9 to 4.3) and 20 to 27 percent by weight of dry substances, is stored air-tightly at a non-elevated temperature, where it is stable for at least a year. The concept “air-tightly” refers to the pulp being stored in e.g. plastic bags or tubes having a volume of 50 to 200 m
3
, or a sealed flat silo.
Said stable pulp is preferably prepared from pulp which has been pressed without lime or aluminium addition. The composition of stable pulp is typically: cellulose and lignin about 30 percent by weight, hemicellulose about 70 percent by weight, of which a third is pectin, pH about 4. This raw material is available throughout the year, its preparation is inexpensive and storage easy. The composition of the raw material is advantageous since it does not include low molecular weight sugars, saccharose or glucose.
REFERENCES:
patent: 4831127 (1989-05-01), Weibel
patent: 5008254 (1991-04-01), Weibel
patent: WO 8403286 (1984-08-01), None
patent: WO 9730215 (1997-08-01), None
STN International, File CAPLUS, CAPLUS accession No. 1983:33388, Prikryl, Jaroslav et al: “Use of preservatives in agriculture. III. Use of silko in the preservation of green forage and sugar beet pulp” & Agrochemia (Bratislava) (1982), 22(10), 279-9.
STN International, File CAPLUS, CAPLUS accession No. 1980: 109374, Gerbut, A. Ya. et al: “Characteristics of storage of highly pressed beat pup”,; & Sakh. Prom-st. (1980), (1), 30-3.
Chemical Abstracts vol. 97 (1982), 90747d.
Chemical Abstracts vol. 98 (1983), 33388.
Antila Juhani
Kuusisto Juhani
Lindqvist Irma Christina
Brunsman David
Nixon & Vanderhye P.C.
Sohkar Oy
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