The method of obtaining maltol from the abies needles

 

(57) Abstract:

The invention relates to the forest industry, in particular to the processing of waste timber industry - fir tree green, and may find application in the cosmetic, food, pharmaceutical, medical industries, and relates to a method of obtaining maltol high purity. The method of obtaining maltol by processing the Abies needles includes its extraction, settling extract, separating the crystalline part from proektirovanii wood greenery and subsequent processing of the last feed on flour and differs in that the assertion of the extract is carried out at a temperature 2-24oC for 16-24 h, the crystalline part after separation was washed with monopolarly organic solvent at a ratio of substance : solvent equal to at least 1:4, then from the crystalline parts of distilled monopolarly organic solvent and sublimation at 95-105oAnd atmospheric pressure produce crystals maltol. The extraction of the Abies needles produce liquid carbon dioxide. The resulting maltol has a purity of 98-99,9%. In the process of paliwanag wood green. 1 C.p. f-crystals, 3 tables.

The invention relates to the forest industry, in particular to the processing of waste timber industry - fir tree green, and may find application in the cosmetic, food, pharmaceutical, medical industries.

The green wood of various species of fir growing on the territory of Russia, is used for the industrial processing of obtaining on picturing installations fir oil, aqueous extract, fish meal, carbon dioxide extract. It is known that extracts from different parts of the fir contain biologically active compounds and, in particular, maltol, which can find application in various industries. Malitol can be used in the food industry to kill the bitterness, improving the taste and smell of food.

The selection of maltol hampered by the fact that it is soluble in polar solvents and easily distilled at a temperature below 100oIn normal conditions, i.e. at temperatures close to the boiling point of the solvent.

A method of obtaining maltol (EN 2047608, C 07 D 309/40, priority from 18.11.93 year). It allows you to get maltol of the es Sibirca shredded Astrovirus of miscella, filtered. The residue after filtration is mixed with silica gel in a mass ratio of 1: (1: 2) and sublimate into the air stream at 140-160oC for 6-7 hours. The disadvantage of this method is that there is a loss maltol that affects the output maltol.

The problem to which the invention is directed, is the further improvement of the method of obtaining maltol with high product yield.

The problem is solved as follows.

The method of obtaining maltol from the Abies needles includes its extraction with carbon dioxide, the defending extract, separating the crystalline part from proektirovanii wood greenery and subsequent processing of the last feed on flour and differs in that the assertion of the extract is carried out at a temperature 0-25oC for 20-24 hours, the crystalline part after separation was washed with monopolarly organic solvent at a ratio of substance : solvent equal to at least 1:4, then from the crystalline parts of distilled monopolarly organic solvent and sublimation at 93-105oWith under reduced atmospheric pressure produce crystals maltol. Extrage">

When implementing the proposed method of fir greens you can get the following products: maltol, carbon dioxide extract, feed flour or compost from proektirovanii wood green.

Extraction of wood greenery carried out in a flow-type apparatus at ambient temperature and corresponding pressure at which carbon dioxide is in a liquid state. At room temperature 18-25oWith the pressure of carbon dioxide (carbon dioxide) is 52-60 ATM. Proektirovanie carbon dioxide extractive substances from the extractor is sent to the collection extractives. The collection is equipped with a jacket for filing deaf steam or warm water. The temperature in the collector extractives should be sufficient to move the liquid carbon dioxide in a gaseous state and under the above conditions is 40-50oC. rise in temperature above the transition point in a gaseous form of carbon dioxide is desirable due to the impact of temperature on biologically active and volatile substances of the extract, flow, necessary to create a large pressure or significantly reduce the temperature when the carbon dioxide of the gas is formed, and is condensed in the condenser of the refrigerator. Under these conditions, the temperature of cooling water for supply to the refrigerating condenser is +(5-15oC). At lower temperatures (higher temperatures in the collection of the extract or the environment, low pressure carbon dioxide) requires the use of cooling agents (salt solutions) and set to cool.

After extraction, the extraction time 3-8 hours) extractor and collector of the extract is separated from the lines of gaseous and liquid carbon dioxide. The extract obtained "perelavlivaet" and freed from carbon dioxide in the receiver of the extract. The extractor release from proektirovanii fir tree green and further processed to feed the flour in a known manner.

Received fodder flour proektirovanii the Abies needles is of higher quality compared to feeding flour derived from wood green in other ways, and approaches the performance vitamin flour fresh woody herbs (see tab. 1).

The higher content of carotene and chlorophyll is explained by extracting features of the liquid carbon dioxide compared to other body is th extraction from wood green highlights water-soluble components (sugar, amino acids, soluble proteins), some components of the wood green denaturised from exposure to high temperature (proteins), which lowers the nutritional value of the flour obtained from proektirovanii wood green. Steam distillation of essential oils of fir tree green also negatively affects the quality of fish meal. Because of the high process temperatures nonremovable ferry carotene and chlorophyll are changed (destroyed), denature proteins, and carbohydrates are extracted with water or caramelicious.

The obtained carbon dioxide extract defend at a temperature of 0-25oC for 20-24 hours. The preferred temperature assertion is the ambient temperature, since at temperatures above the environment requires heating a mixture that will affect the content of biologically active substances in the extract, i.e., will increase the solubility of maltol and energy costs. Lowering the temperature of the settling below the 0oWith will also require energy costs, will reduce the viscosity of the extract and, accordingly, will increase the time of sedimentation of the crystals, and additional contamination of the crystals maltol other compounds (polar acids, waxy connect the rise time settling for more than 24 hours increases the yield of crystals. Defending extracts at a temperature of 2 and 22oWith in 48 hours increases the yield of the crystals 8 and 13%, and within 72 hours of 12 and 15%, respectively, compared to the upholding of the extract for 24 hours at the same temperature.

The separation of the crystalline part of the extract can be siteniravam, by decantation, draining extract through the outlet device located in the sump above the crystals, or by filtration with suction of the liquid portion of the extract. The latter method is preferable because of ease of operation and equipment design, a more complete separation of the crystal from the liquid portion of the extract, the possibility of washing the crystalline part of the filter.

The crystalline part of the extract is washed monopolarly solvent not dissolving or partially dissolving maltol solvent with a low boiling point.

Best for washing the crystals maltol the extraction solvent is benzene, petroleum ether, pentane, hexane, nefras. The temperature of the solvent for washing method and a washing step of flowing or portions washing on the filter, decantation after mixing or infusion) is practically the Asti must be at least 4:1. Reducing the amount of solvent taken to the washing of the crystals, reduces the degree of purification from related substances, which affects the reduction of the yield of crystals maltol at the next stage - the sublimation of maltol. Due to the low solubility of maltol in hydrogen solvent volume increase last taken for leaching (e.g., 60: 1), to the output of maltol no effect. The leaching before sublimation of the crystalline part of the extract is required. Volatile ingredients associated Malcolm substances reduce its output, and volatile substances (essential oils, components of turpentine) reduce the degree of purification due to the joint allocation during sublimation of maltol. The influence of some factors on the degree of purification of the crystalline part of the extract, and the output of maltol are given in table. 2, 3.

From the data table. 2 and 3 it follows that the ratio of substance : solvent 1: 4 allows you to extract only about half of all impurities present in the crystal part. The increase in the ratio substance : solvent is from 1:8 to 1: 60 practical value does not have to extract impurities from the crystalline part. Also no significant values method of washing and the temperature of the solvent, taken the utter 93oC. for the purpose of intensification of the process of the preferred temperature of sublimation is 93-105oC. At higher temperatures the process is resinification product and the decrease in the output of maltol probably because of its high reactivity. The lowering of atmospheric pressure (sublimation under vacuum) allows to increase the output maltol by reducing temperature effects.

Example. Shredded wood green fir in the amount of 7.0 kg were extracted with liquid carbon dioxide at temperature 24oC and a pressure of 56 psi for 5 hours.

Obtained in the separator extract predavlivali in the sump and defended within 24 hours. The resulting crystalline portion separated on the filter from the liquid portion of the extract at the end of the filter remains of the extract was aspirated under reduced pressure 600 mm RT.article (68 kPa) for 10 minutes. Selected crystals were washed with warm (40o(C) petroleum ether (boiling within 40-70o) in the ratio of substance : solvent 1:10. At the end of the leaching has also created negative pressure (68 kPa). The petroleum ether from the extracted part of the drove, got 235 from the crystalline part of Neleus Oleinik ether crystals are transferred into the chamber of sublimation of maltol. Capacity with crystals heated to a temperature of 105oWith, the installation gave a weak current of air supplied to the cooling surface temperature 15oC.

Selected crystals were removed from the cooling surface. The crystals had so pl. 160oC.

The invention will find application in the timber, food, and medical industries, where it is necessary to obtain and apply maltol.

1. The method of obtaining maltol from the Abies needles by extraction with carbon dioxide, settling extract, separating the crystalline part from proektirovanii wood green, sublimation and subsequent processing proektirovanii green feed on flour, characterized in that the assertion of the extract is carried out at a temperature 0-25oC for 20-24 h, the crystalline part after separation was washed with monopolarly organic solvent at a ratio of substance : solvent equal to at least 1: 4, then from the crystalline parts of distilled monopolarly organic solvent and sublimation at 93-105oWith under reduced atmospheric pressure produce crystals maltol.

2. The method according to p. 1, wherein

 

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, (а1), (а2),

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