FI116898B - An improved method for recovering hydroxymatairesinol - Google Patents

Description

IMPROVED METHOD FOR THE EXTRACTION OF HYDROXIMATEIRES

This invention relates to an improved method for the extraction of hydroxime from twigwood in a chip stream by extraction by means of a polar solution. The improvement consists in a more efficient and more feasible method for a of twigwood in the wood material favoring the extraction.

BACKGROUND

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Hydroximatairesinol is an antioxidant lignan, which has been found to have valuable therapeutic properties, including as anticancer agents, as agents for inhibiting certain hormone-dependent diseases and cardiovascular diseases In addition, it has been found that ingestion of hydroxymatairesinol raises serum enterolactone levels, which in turn leads to a number of positive therapeutic effects such as improved cancer protection, see WO 00 59946, Hormos Nutraceutical Oy Ltd It has therefore been proposed to use hydroxymate as a drug or as a supplement to the diet either in the form of a functional food or in the form of a unit dose (capsule or the like) intended for use alongside the daily food. . Patent Publication WO 03/045376, Hon • ♦: Nutraceutical Oy Ltd. further describes the use of e.g. hydroximatai: as an effective agent for suppressing overactivity of certain cell types, i. certain m * * phagocytes and T lymphocytes, thereby preventing the onset of a range of diseases. In addition, it has recently been thinned that hydroximatairesinol is a starting substance for the synthesis of other therapeutically valuable lignans such as matairesinol (WO 03/057209, Hormos Nutraceutical Oy Ltd.), secoisolaric and cyclolariciresionol (WO 03 / 059340, Hormos Nutraceutica • ♦ • · *** T f / 1 \ 45% «· / 4a ·» »X · * rt4 + ^« 11 tiai · irawf iti 2

Substantial levels of hydroximatairesinol have been found in coniferous woods, mainly gn The hydroximatairesinol content is particularly high in twig (twig nuts). The hydroximatairesinol content of the twigs of Nordic spruce (Picea abies I was found to be 5-7% of the twigs.

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Spruce, and especially spruce nuts of spruce wood, are therefore a particularly good fox for hydroximatine resin extraction. Patent Publication WO 03/044004, Ho Nutraceutical Oy Ltd, discloses a process for extraction of hydroxymatore finely divided wood extracted with a polar solvent, such as alcohol and complexing agents added to the extract, whereby hydroxymatairesinol is precipitated in complex form. According to an advantageous embodiment, the wood material is enriched with regard to branch nuts. One such enriched material, which rises at the front pulp, is the fraction of oversized chips which rises at the chipping and subsequent sorting and which, in pulp production, are attempted to enter the pulp as a result of its negative effects] pulp quality. This fraction of oversized chips, which can amount to approx. In practice, 5% of the chips are often led to combustion.

The fraction of the larger chips contains 10-30% twig, which is rich in hydroxamate resinol, and the remainder consists of normal wood. Running the fraction in • # • m 9 · chips directly to combustion means that considerable quantities of raw material in the form of n [wood are often lost for pulp production. Using the fraction supersaturated. The seed for hydroxymatine resin extraction, although technically feasible, constitutes a load on the extraction process, since only approx. 30% of the wood material to be extracted contains greater amounts of hydroxymatairesinol. Andelei ... normalwood is only a burden for the extraction process at the same time s <* · * ..! share vote a valuable supplement to the pulp industry.

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Separation Research Ltd., describes such a process. The fraction is overfished or an air-sifted, heavy fraction thereof is ground into sticks, after which the sticks are dried and then mixed with water, whereby the sticks are separated into a light fraction and a heavy fraction (the sediment) by means of a vat. The sediment sticks are rich in extractives and are led to extraction, while the light fraction, which largely consists of normal wood, is intended to be guided to the pulping process.

The above described fractionation process, however, associated with a number of disadvantages - the drying of the wood material prior to separation constitutes an energy consuming pathway - the wet sedimented material to be used in the extraction (which in practice is not suitable to integrate with the pulping process) is not as storage-resistant, but requires separate drying - the sedimented twig-containing material must also be dried before extracting - the moisture content of the wood material recycled to the pulping process fluctuates <from the moisture content of the main stream of the chip material - water-based sedimentation process is a unitary process which is unitary

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: SUMMARY OF THE INVENTION

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The object of the present invention is to provide an improved extraction method for the extraction of hydroxymatairesinol from twigwood derived from the flow of oversized chips in connection with a pulping process. The improvement applies. fractionation of the oversized chips. In the fractionation according to this invention, an attempt is made to achieve an improved, non-water-borne process. , m 1J1 1 j,. * 1 * | | 4 b) the finely divided material from step a) is separated without prior drying and / or mixing with water in a light fraction and a heavy fraction, c) the heavy fraction from step b) is extracted with a polar solvent d) hydroxymatrazinol is recovered from the extract .

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BRIEF DESCRIPTION OF THE FIGURES

Figure 1 shows schematically a known method for enriching twig material chip flow,

Figure 2 schematically illustrates a process for extracting hydroxymatrizin twig from a stream of oversized wood, where the flow of material guided to the extraction is enriched for twig according to the present invention. Figure 3 shows an alternative embodiment of the method according to the invention.

Figure 4 shows another alternative embodiment of the method according to the invention

Figure 5 shows a third alternative embodiment of the method according to the invention - 20 a w

*: · DETAILED DESCRIPTION OF THE INVENTION

Figure 1 describes the water-based process for enriching twig nut * * a chip stream according to FI20001739. According to the figure, it is an air-sifted fraction of the larger chips that is taken into atomisation, but alternatively, the total fraction of the chips can also be led to atomisation, subsequent drying, mixing and water-based sedimentation. If air sieving is used, it is at least 5 fold distribution that is elevated if viewed from the point of view of extraction. At the same time, to ensure that the portion of the comminuted material which the pulping process is of good quality for pulping, it is desirable to use such a comminution which removes thin sticks but which substantially cuts the fibers in their longitudinal direction. Examples of such particle distribution processes may be mentioned the "pin chips" process, which is normally a for the atomization of the oversized chip in the manufacture of mechanical pulp examples of suitable atomizers, the devices described in US 5,937,923, US 4,235,382 and US 4,953,795. Another ex-conceivable atomizer is e.g. a pinwheel, e.g. a swab of / described in Russian Patent FI105699.

After the atomization, the material is conducted without prior drying and / or water slurry for separation. The purpose of the separation step is to divide the finely divided material into a twig-rich fraction and another fraction with or lay hait of twig wood. It has been found that the chunky chips have a higher weight than chips with a low twig content. Therefore, it is also possible to formulate the purpose so as to strive to subdivide the finely divided material into a heavy (i.e., twig-rich) fraction for the subsequent extraction and the hydroxime resin extraction and a light fraction, as if it has a lamp. • · · · 1 | fiber quality, is fed back to the pulping process, or if the quality requirements are not up; ·····] is led to other uses (eg combustion).

* * ·· * * · · \,; The separation can be carried out in many alternative ways. For example, nam * * * * * can be air separation (ADS) described e.g. in US and US 5,829,597 Beloit Technologies Inc. and US 6,283,300. The principle * · I *.! the finely divided material is led into an empty area where an eaten “....... ......

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The separation into a heavy fraction and a light fraction does not necessarily require a unit operation that utilizes differences in specific weight of the material thus separated. It is known from experience that twigs are much more difficult to refine normal wood. By using a conventional sorting based on the particle size (grating, disk strainer, for example, according to FI92476 or closing strainer, eg according to 101203). The suitability of a sorting based on particle size depends on the atomization technique used.

Figure 3 shows an alternative procedure in which the oversized chips are sorted in an air sieving step, after which only a branch-rich fraction of the material is led to atomization and further processing.

Figure 4 shows a third alternative, where at least part of the heavy fractional separation step is led back to the preceding distribution stage.

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Figure 5 shows a fourth alternative where there are two consecutive atomisation and separation steps.

The method according to the invention does not limit itself to the above-described, with the described embodiments. It will be obvious to those skilled in the art that modifying j.i: and combinations may be used. Thus, the combining processes of Figures 4 and 5 can be increased, the number of atomisation and separation steps increased and * linked together in different ways. Furthermore, it should be noted that one of the figures in the *****: atomisation or separation steps can itself consist of two or more different ***** * · · · 25 successive and / or parallel unit operations. The comminution and separation process can, of course, be firmly integrated into the pulp milling process. Alternatively, one can think that eg the same or different light transportable, e.g. wheeled support, which can be transported by car to the desired location.

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Summary of the Advantages of the Process of the Invention: - The treated wood material taken for hydroximetry resinole extraction of high content of twig material, thereby saving chemicals and engineering costs in the form of appliance equipment for the extraction stage as less wood consuming material is used and energy consuming separates are avoided - the single-poured twig-rich wood material has not been exposed to moisture but is resistant to storage and can be used for extraction at the desired location and we suitable time 15 - the appliances are of the accepted type and easy to integrate into the pulp-handling process in pulp-mill material as usual without precedence - the device for atomizing and separating the wood material to be extracted can easily be built as a portable unit ·· ♦ * * · · * II »i}> · a» a »• 4 * • • i 4» * I · I a »• * * • 4 • ·« a 4 4 · 4 · * • 4 · 4 t • f 44 · • · 4 | 4 4 »

Claims (7)

A method for recovering hydroxymatairesinol from a branch tree of a material stream of excess chips, characterized in that 5 a) the chips or fraction fractionated in the air stream thereof are comminuted; and / or mixing with water a light fraction and a heavy fraction, c) extracting the heavy fraction obtained in step b) as a polar solvent, and d) recovering the hydroxymatairesinol from the extract. Process according to Claim 1, characterized in that the heavy fraction from step b) according to claim 1 is, in turn, re-sorted without prior drying and / or mixing1 to a light fraction and a heavy fraction, followed by extraction of the latter fraction with a polar solvent. A process according to claim 2, characterized in that the heavy fraction from step b) according to claim 1 is, in turn, re-sorted without prior drying and / or mixing1 to 20 lightweight and heavy fraction such that at least a portion of the 1, the heavy fraction from step b) is exported or treated with heavy chips or heavy air sorted in its air stream. • t i • · · • ♦ • ♦ ··· The process according to claim 2, characterized in that the heavy fraction from step b) according to claim 1 is refined in turn without any previous drying and / or mixing a e · B ·. . π A method according to any one of the preceding claims, characterized in that the sorting according to claim 1 step b) into a light fraction and a heavy fraction is a particle size sorting, air stream sorting or cyclone treatment, or a combination thereof. 5 Process according to any one of the preceding claims, characterized in that an agent capable of complexing with hydroxymatairesinol is added to the extract or concentrated fraction thereof and the hydroxymatairesinol is recovered in the form of a precipitated complex. 10 7. A device for enriching a branch from a stream of heavy fraction sorted by its overflow chips, characterized in that it comprises at least one rabbit and at least one sorting device for sorting the material coming from the crusher without drying and / or mixing with light both the comminuting device and the sorting device are mounted on one or more transportable substrates. m · · • 1 «·« ·· • φ • · φ f «i« · «♦ • • · ΨΨ # • 1 1 * · * ·· • 1 • · * ·« • φ • · φ • · «1 · φ · 1 • · * φ