CS270904B1 - Method of oligosaccharides,glucose and hydrolysates of starch cleaning - Google Patents

Abstract

This solution relates to a method of the purification of glucose, oligosaccharides and starch hydrolysates in various technological phases by means of cellulose ionex derivatives. The method of purification of oligosaccharides, glucose or starch hydrolysates solutions rests in the fact that 40 up to 100 parts of the solution get in contact with 1 part of pearl cellulose containing (N,N-diethyl)amine groups in OH- or Cl-form in a mixing tank or packed column, in a concentration of up to 1.1 mmole/g, or with the pearl cellulose regenerated by washing with 3 mass parts of salt solutions or the basis selected from the group containing sodium chloride and potassium hydroxide with a concentration of 0.5 to 1 mole/1 with subsequent washing by the same volume of 1 mole/1 of hydrochloric acid and/or distilled water to the maximum. This purification method can be performed either in continuous or discontinuous equipment while the sorbent is recoverable. In this way, the starch or glucose solutions of various origins can be purified at variant technological phases.

Description

(57) The present invention relates to a process for the purification of a solution of glucose, oligosaccharides and starch hydrolysates at different technological stages using ion-exchange cellulose derivatives. A method for the purification of glucose oligosaccharide solutions or starch hydrolyzates is to contact 40-100 parts of the solution in a stirred vessel or packed with a β 1 column with a portion of pearl cellulose containing (N, N-diethyl) amino groups in OH or Cl form at a concentration of up to 1.1 mmol / g, optionally with 6 pearl cellulose regenerated by washing with 3 volumes of salt or base solutions selected from the group consisting of sodium chloride and potassium hydroxide at a concentration of 0.5 to 1 mol / l followed by washing with the same a volume of not more than 1 mol / l hydrochloric acid and / or distilled water. Thus, this purification process can be carried out in both continuous and discontinuous equipment, the eorbent being regenerable. In this way, starch or glucose solutions of different provenance can be purified at different technological stages.

1270 904 Italy (11) (13) Bl (51) Int. Cl. ⁵ C 13 К 1/00

CS 270 904 B1

AND

The invention relates to a process for the purification of glucose solutions, oligosaccharides and starch hydrolysates at various technological stages by means of ion-exchange cellulose derivatives.

The current method of purifying glucose solutions prepared by hydrolyzing liquefied starch ion exchange resins (as follows from a computerized search in the Chemical Abstracts and World Patent Index (WPI) between 1960 and 1984) is to use a strongly acidic cation exchange resin. from starch (NG Gulyuh: USSR Pat. 207824 (1966), Chem. Abstr. 69, 20603 (1969)). However, strongly basic anion exchangers with polymeric sorbents without macroporous type ionogenic groups are also proposed for this purpose, in particular for the purification of eacharose (št. Stamberg, V. Valter: Entfarbungsharze, Akademie-Verleg-Serlin (1970)). In practice, however, starch hydrolysis solutions are purified by mixing with carbrafline, filtration, and the isolated glucose is crystallized twice. The disadvantages of carboraffin purification are poor filterability, difficulty in removing adsorbent from solution and adsorbent collection.

These disadvantages are overcome by a process for the purification of starch and glucose solutions, wherein said solutions are contacted in bead cellulose with diethylamine or 1- (N, N-diethylamino) -2-hydroxypropyl groups. The aforementioned purification method can advantageously be carried out by passing the solution through a layer of cellulose derivatives in pearl form.

An advantage of the process according to the invention is that it can be carried out both batchwise by loading ion-exchange cellulose into a starch or glucose solution, and continuously by flowing the solution through a column packed with pearl cellulose. Compared to purifying solutions in a batch-like manner in a tank, the column method is more efficient. However, the first method does not require any additional devices. It should be emphasized here that the sorption proceeds even at an elevated temperature of 25 to 95 ° C.

The basic prerequisite for this method of cleaning is sufficient strength and incompressibility of the carrier. However, pearl cellulose is sufficiently abrasion resistant.

SUMMARY OF THE INVENTION The present invention provides a process for the purification of glucose oligosecharide solutions or starch hydrolyzates comprising contacting 40-100 parts of a solution in a stirred vessel or packed column with 1 part pearl cellulose containing [N, N-dimethyl] amino groups in OH or Cl form at a concentration of up to 1.1 mmol / g, optionally with pearl cellulose regenerated by washing with 3 volumes of salt or base solutions selected from the group consisting of sodium chloride and potassium hydroxide at a concentration of 0.5 to 1 mol / l subsequent washing with an equal volume of max. 1 mol / l hydrochloric acid and / or distilled water.

Thus, this purification process can be carried out in both continuous and diisocontinuous equipment, the sorbent being regenerable. Regeneration is performed by washing three times the volume of a bed of a salt or base solution selected from the group consisting of sodium chloride and sodium hydroxide up to a concentration of 1 mol / l, followed by washing with an equal volume of up to 1 mol / l hydrochloric acid and distilled water. The starch or glucose solutions of various provenance can be purified at various stages of the process according to the invention. Thus, potato, corn or other starch solutions can be purified. Furthermore, the starch solutions after liquefaction or preferably after hydrolysis, i.e. glucose syrup. The degree of purification of the solutions was monitored by measuring the absorption of the solutions at 280 nm, where the absorption maximum of the solutions was found.

The higher effect of the process according to the invention lies primarily in the high sorption ability of pearl cellulose with diethylamine groups to the coloring substances contained in starch and glucose solutions. The higher effect further consists in the regular spherical shape of the proposed sorbent, which allows rapid filtration due to low layer resistance and the fact that these particles do not abrasion when compared to carboraffin, in the possibility of regenerating the sorbent by de-adsorption of colored substances.

CS 270 904 81 with a salt or base solution such as 1 mol / l sodium chloride and 1 mol / l sodium hydroxide, respectively.

The examples below illustrate a method for purifying solutions without limiting the scope of the invention.

Example 1 parts of liquefied potato starch (27.9 wt%, dry matter, glucose equivalent of 23.2) was pumped at 50 ° C through 1 part of bead cellulose containing 1- (N, N-diethylamino) -2-hydroxypropyl groups in a concentration of 1.07 mmol / g granularity of 0.3 to 1.0 mm in Cl form placed in a column of 3 cm length and 1.5 cm diameter at a rate of 0.25 parts / min. The absorption maximum change at 280 nm continued to trap 35% of the mass of the colorants.

Example 2 parts glucose syrup (29.5 wt%, dry matter, glucose equivalent 97.8) was pumped at 50 ° C through 1 part pearl cellulose containing (N, N-diethylamino) ethyl groups (1 mmol / g) in Cl form speed 0.46 parts / min. According to the change in the abeorption maximum at 280 nm, 43% by weight of color substances were removed from the glucose solution by flowing through the ion exchanger. Under dynamic conditions, when the bead cellulose was placed in the column, no loss of column pressure or layer compressibility up to 20 kPa was observed.

Example 3

In 50 parts liquefied corn starch (35.2 wt%, dry matter, glucose equivalent 30%), 1 part pearl cellulose with 1- (N, N-diethylamino) -2-hydroxypropyl groups (1.08 mmol / g) was mixed in the flask. (grain size 0.135-0.44 mm) at 70 ° C. After 30 minutes of contact with gentle agitation with an anchor stirrer (100 rpm), the absorption of the solution at 280 nm was 26% lower than the original solution and its foaming was removed. Of the liquefied corn starch, the absolute highest amount of impurities was absorbed, which was almost 200% (2 x) of the impurities sorbed from glucose syrup and 120% (1 x 2) of impurities in the liquefied potato starch.

The sorbent was recovered in the column after the sorption by flowing 0.1 and 1.0 mol / L sodium chloride, hydrochloric acid, and sodium hydroxide solutions. At desorption of 0.1 mol / l sodium chloride, 30% by weight of sorbed substances, 1.0 mol / l sodium chloride 29% by weight, 0.1 mol / l hydrochloric acid 7% by weight, 1.0 mol / l are absorbed. 1% hydrochloric acid, 8% by weight, 0.1 mol / l sodium hydroxide 15% by weight, and 1.0 mol / l sodium hydroxide 9% by weight, of the sorbents. Regeneration was terminated by converting to Cl-form 1 mol / L hydrochloric acid and washing with distilled water to neutral. After regeneration, the ion exchanger used absorbed the same amount of colored substances.

Example 4

The procedure described in Example 2 was used to purify the glucose syrup purified before that with carboraffin. However, the bead cellulose in the diethylamine groups from this solution absorbed an additional 26% by weight of coloring substances, as measured by the absorption at 280 nm.

Example 5

As described in Example 2, 100 parts of glucose syrup, 1 part of pearl cellulose and diethylamine groups were purified. From this solution, a proportion of additional% of the colorants absorbed as measured by the absorbance at 280 nm, which decreased by 26%.

The bead cellulose was regenerated by washing 1. 1 part of a 0.5 mol / l sodium chloride solution or 0.5 mol / l sodium hydroxide and 2 parts distilled water.

CS 270 904 Bl

Claims (1)

BACKGROUND OF THE INVENTION A process for the purification of oligoeacharide, glucose and starch hydrolyzates solutions characterized by: characterized in that 40 to 100 parts of the solution are contacted in a stirred vessel or packed column with 1 part of pearl cellulose containing (N, N-diethyl) amino groups in OH or Cl form in a concentration of up to 1.1 mmol / g, optionally and bead regenerated by washing with 3 volumes of salt or base solutions selected from the group consisting of sodium chloride and potassium hydroxide at a concentration of 0.5 to 1 mol / l followed by washing with an equal volume to 1 mol / l hydrochloric acid and / or distilled water .