Birch bark processing method

FIELD: wood-working and wood chemical industry.

SUBSTANCE: proposed method of birch bark processing includes crushing birch bark in crusher; separation into silver bark and bast: extraction of silver bark using solvent in form of zeotropic mixture of tetrachloroethylene and water; separation of solution from cake; separation of precipitated crystals from mother liquor, washing of crystals with subsequent drying of received product - mixture of three-five triterpene compounds; boiling down of mother liquor to get dry remnant, washing the latter in distilled water with subsequent drying of obtained product - mixture of five-seventeen triterpene compounds; removal of solvent from said cake by mixing it with water and subsequent boiling down of mixture for complete removal of solvent; mixing of said cake with sodium hydroxide and isopropyl alcohol, boiling of said mixture, separation of solution from undissolved sidement, washing of undissolved sediment with distilled water and subsequent drying of obtained product - ligning; distillation of isopropyl alcohol from filtrate, acidification of remaining solution to pH=4.5 - 5.5 and holding it at temperature from minus 5 to 25°C for 0.5-15 h. separation of precipitated sediment from solution, washing of sediment with subsequent drying of obtained product - birch wax; crushing of bast, mixing of bast particles with water, holding of mixture for 1-20 days, separation of sediment from obtained product - sour compound; drying of sediment which can be used as feed additive for cattle and poultry.

EFFECT: provision of complex processing of birch bark.

24 cl, 3 ex, 2 dwg

 

The invention relates to woodworking and timber industry and can be used to extract valuable chemicals for cosmetics, pharmaceutical and medical industry of waste wood, in particular betulin formula (1) from birch bark, which is a waste product of the plywood and pulp and paper enterprises.

Currently, the bark is removed and stored in dumps. Only one pulp and paper mill blade bark annually replenished by 50 thousand tons. Birch bark consists of two components: the outer layer of birch bark and the inner layer of bark. Elm is a durable multi-layered cork fabric, chemical components which are extracted by organic solvents are substances of class triterpenes, including triterpene diatomic alcohol betulin, representing a white crystalline powder with a melting point 251-252°C.

In addition betulin elm contains suberin (polyostotic irregular structure), available polyphenols, lignin and polysaccharides. The phloem is a tissue consisting of sugars, easily and trudnoizvlekaemyh polysaccharides, lignin, tannins and other compounds. Because of the presence of Beresta large number of triterpene compounds, preventing rot, birch bark resists decomposition for a long time and is not suitable for industrial processing unprepared, as a result of its dumps occupy large territories and are dangerous for the environment.

A method of obtaining natural derivative compounds from birch bark (see US patent No. 6280778, IPC AC 35/78, published 28.08.2001, including the soaking bark for from 1 minute to 24 hours at a temperature of from 80°160°composition: organic solvent, extracting natural compounds from birch bark, and chemically active reagent. As the organic solvent used chloroform, CHCl3, dichloromethane CH2Cl2, diethyl ether (CH3CH2)2O, tetrahydrofuran, acetone, pyridine and dimethylformamide DMF. As a chemically active reagent use nitrates of iron, copper, chromium, zinc, mercury, selenium, manganese, silver, chromium oxide; the chlorides of iron, silver; pyridineboronic RCC, pyridinediamine PDC, K2FeO4, K2MnO4, KMnO4, BaMnO4, AgCO3, RuCl3and several others.

There is a method allows one process to obtain various derivatives of betulin or lupeol. The disadvantage of this method is the use of chemically active reagent in achiev is Tate which wastes require disposal of special polygons, the method is complex, characterized by a low yield of product.

A method of obtaining betulin from birch bark (see patent RU No. 2172178, IPC AC 35/78, published 20.08.2001, including the shredding bark, split bark on bark and phloem, the extraction of birch bark 90-95% ethyl alcohol with a temperature of 70-75°with the addition of activated carbon, separating the solution, followed by removing the solvent.

The disadvantage of this method is not a high quality betulin, a large amount of waste.

A method of obtaining betulin from birch bark (see patent RU No. 2264411, IPC C07J 53/00, published 20.11.2005, including the shredding bark, processing shredded bark with a mixture of water-alcohol-alkali when using the shock-acoustic stimulation for 5 minutes at a temperature of 70° (C), evaporation of the resulting solution, the precipitation of betulin from one stripped off solution upon dilution with water and subsequent separation of betulin filtering.

Shock-acoustic activation intensifies the hydrolysis of birch bark, which in a few minutes turns into a homogeneous mass of brown. However, when the shock-acoustic activation forms a homogeneous mass is subjected to filtration. Besieged betulin contaminated difficult detachable alkali. Itself the shock-acoustic is Skye activation harmful for staff, besides, not provided full use of the components of the bark.

A method of refining birch bark for obtaining betulin (see patent RU No. 2234936, IPC AC 35/79 published 27.08.2004, including the shredding bark, split it on the bark and phloem, the extraction of birch bark by pouring her 1-butanol and exposure within 2-48 hours at a temperature of 20-120°, filtering the resulting solution, the Stripping of the solvent, the extract residue for 2-16 hours at a temperature of 5-15°for crystallization betulin, filtration of the crystals betulin, spin on filter, washing with water and drying. Mainly bark and 1-butanol take in a ratio of from 1:1 to 1:10.

The known method provides the output of the weight of the dry bark of 45 wt.% betulin 98%purity. The disadvantages of this method include an excessively large duration of exposure, the use of expensive solvent, the impossibility of obtaining pure betulin in one stage.

A known method of extraction of betulin (see patent RU No. 2206572, IPC C07J 53/00, published 20.06.2003,), which separates the bark from the bast, bark crushed with a rotary knife mill, a fraction of 0.5-5.0 mm extracted with hexane in 3-5 hours. The extract obtained was washed with distilled water, after separation falls crystalline precipitate containing 92-97% betulin. Then the water on the make from the extract. The precipitate is filtered off and dried. The output of this product is 5-8% by weight of air-dried bark taken for extraction (stage I). Next, the extract evaporated, which results in a precipitate triterpene compounds, the main of which is betulin, and the resulting solvent return for the next extraction process. The precipitate is washed with water and dried. The output is 15-20% by weight of the extracted product with a basic substance content of 60-70% (stage II). In the known method without additional purification receive a product containing 92-97% betulin reduction of the time of extraction.

In the known method the separation of the bark from the bast requires the use of manual labor, and the process of selection of betulin is quite complex.

A method of refining birch bark for obtaining betulin (see patent RU No. 2192879, IPC AC 35/78, published 20.11.2002,), coinciding with the inventive solution for the greatest number of significant features and adopted for the prototype. The method includes grinding the bark on the crusher, the division into the bark and phloem, the extraction of birch bark toluene by stirring bark with toluene for 1.5 to 3.0 hours at a temperature of 90-110°, filtration of the solution at a temperature of 40-50°C, cooling the solution of betulin in toluene for 6-10 hours until the temperature 15-5° With a stirring precipitated crystals betulin from the mother liquor, filtering, washing with clean toluene, filtration and drying, washing with ethyl alcohol or isopropyl, then with water, and drying.

In a known way as a result of extraction with stirring for 1.5 to 3.0 hours is formed persistent, poorly filterable emulsion, the use of pure solvent increases the cost allocation process betulin, at a temperature of filtering 40-50°betulin begins to fall from toluene, to crystallize in the pipes and clog them. And most importantly, there is a method-prototype does not provide complex processing of birch bark, resulting in the waste is a lot of valuable substances.

The objective of the proposed technical solution was to develop such a method for processing of birch bark, which would provide a comprehensive extract from the bark of commercial products.

The problem is solved by the claimed method including the successive grinding of bark in the crusher; the division into the bark and phloem; extraction of birch bark solvent in the form of an azeotropic mixture of tetrachloroethylene - water for 0.5-1.4 hours at a temperature of 89-115°C, a pressure of 0.1-1.0 MPa; separating the solution from the meal at a temperature of 80-100°s; keeping the filtrate in the mould for 1-5 hours at a temperature of from -5°what about the +25° S; separation of precipitated crystals from the mother liquor; washing the crystals with distilled water or 20%aqueous solution of ethyl alcohol, followed by drying the obtained product is a mixture of three-petiteteenager compounds; the process of evaporation of the mother liquor to obtain a dry residue; rinse it with distilled water, followed by drying the obtained product is a mixture of five-semnadtsatitysyachnyj compounds; removing the solvent from the meal by mixing it with water and subsequent evaporation of the mixture to remove the solvent, mixing the resulting meal with sodium hydroxide and isopropyl alcohol; boiling the mixture for 0.5 to 5.0 hours; separating the solution from nerastvorimogo the precipitate at a temperature of 40-80°s; washing of nerastvorimogo precipitate with distilled water, followed by drying the obtained product of lignin (amorphous powder yellow-brown or brown color); the distillation of the filtrate isopropyl alcohol; the acidification of the remaining solution to pH=4.5 to 5.5 and aging it at a temperature of 5-25°C for 0.5 to 15 hours (at -5°With target product is allocated for 0.5 hours and at +25° - 15 hours); Department of precipitated sludge from solution; washing the precipitate with distilled water, followed by drying of the resulting product - the birch of the wax, as well as from alchemie bast particles of 0.1-5.0 mm, mixing them with water in an amount of 7-10 liters per 1 kg of particles of bast, the extract mixture at a temperature of 15-40°C for 1-10 days, separating the precipitate from the resulting product - the birch of kvass, drying the precipitate, which is added to animal feed for farm animals and birds.

As a result of implementation of the proposed method in addition to a mixture of triterpene compounds, mainly betulin get the lignin, birch wax, kvass and feed additive, it does not use hazardous substances, birch bark is processed and used fully used for recycling the solvent to be regenerated and reused.

Using as solvent tetrachloroethylene, due to its fire - and explosion safety, low toxicity, high solubility of target compounds and insolubility in it ballast substances. It does not form stable emulsions are relatively inexpensive, in contrast to toluene, it is less dangerous for personnel.

The use of azeotropic mixture of solvent and water can reduce the cost of the extraction process without affecting the result.

When the extraction is less than 0.5 hours significantly reduced the percentage of extraction of triterpene compounds and extraction of more than 1.4 hours, especially under intensive stirring, the whole is howling product completely in the extract even at low module and further extraction forms a stable emulsion-solvent-water-betulin (betulin is an excellent emulsifier), further complicating the process.

Extraction at a temperature below 89°does not allow complete extraction of betulin, and at a temperature of more than 115°extraction is not because of the boiling solvent.

Extraction at a pressure less than 0.1 MPa impractical because it leads to large losses of solvent and at a pressure of 1.0 MPa, the process requires the use of expensive equipment.

The separation of the solution from the meal at a temperature below 80°leads to the deposition of the target product in the pipeline, and at temperatures above 100°With the solution boils, which leads to large losses.

During curing of the filtrate in the mould less than 1 hour at a temperature below -5°does not fully highlight the target product, and if the shutter speed is more than 5 hours at a temperature above 15°does not increase the allocation of the target product, resulting to stand next is not advisable.

Boiling a mixture of meal with sodium hydroxide and isopropyl alcohol within less than 0.5 hours is not possible to react the reagents completely and boiling more than 5.0 hours is not advisable, because during this time, the reagents will react completely.

Separating the solution from nerastvorimogo residue (lignin) at a temperature below 40°does not give a complete purification of lignin, and at a temperature of more than 80°to process the e appropriate, as the mixture boils.

Acidification of the solution remaining after separation of lignin, to a pH of less than 4.5 leads to incomplete separation of the target product, and upon acidification to a pH of greater 5,5 excess acid will neutralize at the end of the process.

Extract the acidified solution at a temperature below -5°C for 0.5 hours and more than 15 hours at a temperature above 25°does not increase the yield of target products.

Grinding bast on particles less than 0.1 mm leads to inappropriate energy, and when the particle sizes of more than 5.0 mm worsens the extraction of target products and reduced their output due to incomplete access of solvent.

Adding water in a quantity of less than 7 liters per 1 kg of the particles bast is too concentrated brew, adding more than 10 liters per 1 kg of the particles bast changes the properties of the obtained product.

When the extract of a mixture of water and particles of bast at a temperature of less than 15°slows down the process and, consequently, more expensive, and the shutter speed at a temperature of more than 40°With stops the fermentation process.

Shutter speed less than 1 hour does not ensure the completion of the process of fermentation and aging for more than 10 days leads to acetic acid fermentation and spoilage of the product.

The bark can be removed, for example, debarking machine.

Grinding cor which can be implemented in a knife mill, then using a hammer mill.

Separation of shredded bark on bark and phloem can be carried out on an inclined plane with holes of arbitrary shape, to fit into the circle d 1-15 mm, oscillating in the horizontal and vertical planes with the amplitude of 5-150 mm, a frequency of 1-300 Hz.

Suitable extraction of triterpene compounds to implement when the mass ratio of bark and solvent 1:(2-10). At a ratio less than 1:2 solvent does not cover the bark, and when the ratio is about 1:10 is impeded identification of target product, in this case, the extraction can be carried out as under stirring bark and solvent, and without stirring.

The separation of the precipitated crystals triterpene compounds from the mother liquor can be filtered through a filter with a pore size of from 0.2 to 200 μm (pore size less than 0.2 μm filtration rate almost equal to 0 due to the rapid filling of the pores of the crystals, and when the pore size is more than 200 μm is a great breakthrough crystals, which reduces the yield of the product), and other known methods, such as gravitational settling.

Washing crystals three-petiteteenager compounds distilled water or 20%aqueous solution of ethyl alcohol gets rid of the ballast substances and, most importantly, the residual solvent, and washing crystals five-semnadtsatitysyachnyj compounds, a mixture of lignin, birch wax can be realized in the amount of 1-10 liters per 1 kg of crystals. The smaller the washing liquid is not provided the required purity of the crystals, and greater than 10 liters volume of the washing liquid is not economically feasible.

To accelerate the process of drying the obtained product is a mixture of 3-5 triterpene compounds, mixtures 5-17 triterpene compounds, lignin, birch wax is carried out at a temperature 50-125°and a pressure of from 0.01 to 0.10 MPa as with stirring or without stirring of the product. Drying at a temperature of 50°you must maintain at a pressure of 0.01 MPa and at a temperature of 125°at a pressure of 0.10 MPa, which is caused by the boiling point of the residual solvent in the above pressures. The choice of pressure and temperature is determined by the production capacity.

Preferably the dry cake mix with sodium hydroxide and isopropyl alcohol in the following ratio of components:

sodium hydroxide - 0,10-0,15 kg;

isopropyl alcohol - 2,0-5,0 kg

on 1 kg of dry meal.

Separating the solution from nerastvorimogo in sodium hydroxide and isopropyl alcohol precipitate, from the fall of the acidified solution of the precipitate may then be filtered through a filter with dimensions of the EOS from 0.2 to 200 μm. When the pore size less than 0.2 μm filtration rate almost equal to 0 due to the rapid filling of the pores of the crystals, and when the pore size is more than 200 μm is a great breakthrough crystals, which reduces the yield of the product.

Acidification of the solution remaining after the distillation of the filtrate isopropyl alcohol, need to acetic acid, hydrochloric acid or carbonic acid, as the use of other acids gives a large amount of waste in the form of solutions of salts (sulphates, nitrates) of these acids.

The inventive method is illustrated by drawings, where:

- figure 1 shows the sequence of operations of the proposed method;

- figure 2 shows the continuation of the sequence of operations depicted in figure 1.

The inventive method of processing of birch bark is as follows. After separation of birch bark from wood, for example, using a debarking machine, or any other known mechanism for debarking of wood during the preparatory stage of the production of plywood or pulp, birch bark serves, for example, a conveyor belt or screw, in the grinding device. As the grinding device can be used, for example, hammer crusher with the holes in the grates from 5 to 25 mm and a frequency of rotation the rotor from 900 up to 6500 rpm, korolovka or any other known device for grinding large source material. If the processing of birch bark is not built into the manufacturing process of plywood or pulp and requires delivery by truck or rail, the grinding process is preferably divided into two stages. The bark is advisable to chop in two stages. On first use colorusso or knife grinder without grate to reduce the amount of bark two or three times to reduce transport costs. The second stage crushing crust conduct already in place recycling of crust in a hammer mill. After crushing the bark is divided into components: on the bark and phloem of classifying the device. The separation can be done according to the size of particles, as the particles of bark and bast after grinding are different sizes. To separate particles of bark and bast size can be used vibrating screens or any other known device based on this principle. The separation can be performed also by the weight of the particles, as the particles of bark and bast have different specific weight. For this separation can be used pneumatic classifier or other known device based on this principle. Pneumatic classifier can be constructively is Beginin with shredder (for example, hammer crusher with axial fan on one rotor with hammers). Particles of bark placed in the extractor, which serves azeotropic mixture of tetrachloroethylene - water (boiling point 89-115°). The predominant mass ratio of bark and solvent 1:(2-10). Extraction of birch bark carry out the solvent in the form of an azeotropic mixture of tetrachloroethylene - water for 0.5-1.4 hours at a temperature of 89-115°C, a pressure of 0.1-1.0 MPa. During the extraction mixture for process intensification can be mixed, for example, a mixer. After extraction, separating the resulting solution from the meal at a temperature of 80-100°With, for example, by filtration through the filter surface with a pore size of 0.2 to 200 μm, separation or sedimentation (sedimentation). The filtrate is placed in a mold where was incubated for 1-5 hours at a temperature of from -5°C to +25°C. Further separate the precipitated crystals from the mother liquor, for example, by filtration through the filter surface with a pore size of 0.2 to 200 μm, separation or sedimentation (sedimentation). Wash the crystals with distilled water or 20%aqueous solution of ethyl alcohol. Preferably 1 kg of crystals rinse 1-10 liters of water or 20%aqueous solution of ethyl alcohol. The washed crystals are then dried. To accelerate drying it is conducted at temperatures 50-12° C and a pressure of from 0.01 to 0.10 MPa with stirring, crystals, or without. The resulting product is a mixture of three-petiteteenager compounds, including triterpene diatomic alcohol-betulin (90 wt%), the output from 8 to 15% by weight is loaded into the extractor bark. The remaining mother liquor is evaporated to obtain a dry residue, which is washed with distilled water. It is recommended that 1 kg of dry residue washed 1-10 liters of water. Then dry the resulting product is a mixture of five-semnadtsatitysyachnyj compounds, including triterpene diatomic alcohol-betulin (30-90 wt.%), the output from 5 to 10% by weight is loaded into the extractor bark. To accelerate drying it is carried out at a temperature of 50-125°and a pressure of from 0.01 to 0.10 MPa with stirring of the product. Of meal remaining in the extractor, remove the solvent by mixing it with water, mostly in the ratio of 1 wt. part of the meal 1-10 wt. parts of water. The mixture is brought to a boil, stand up to complete removal of a mixture of water with the solvent. The end of the distillation is determined by the temperature in the extractor to 100°C. In the extractor add sodium hydroxide and isopropyl alcohol at the rate of 0.10 to 0.15 kg of NaOH and from 2 to 5 kg of isopropyl alcohol (preferably hot) to 1 kg of meal, bring to a boil and boil the mixture for 0.5 to 5.0 hours. Then separate rest the R from nerastvorimogo precipitate at a temperature of 40-80° C. separating the solution from the precipitate are, for example, by filtration through the filter surface with a pore size of 0.2 to 200 μm, separation or sedimentation (sedimentation). Washed nerastvorim the precipitate with distilled water, mainly 1-10 liters of water per 1 kg of sediment. Next, the obtained dried product lignin. To accelerate drying it is carried out at a temperature of 50-125°and a pressure of from 0.01 to 0.10 MPa with stirring lignin. From the filtrate distilled isopropyl alcohol, the remaining solution was acidified to pH=4,5-5,5, for example, acetic, hydrochloric or carbonic acid. Withstand the acidified solution at a temperature of from -5°to 25°C for 0.5 to 15 hours with stirring or without stirring (shutter speed depends on the temperature, the higher the temperature, the longer the shutter speed). Next, separate the precipitation from solution, for example, by filtration through the filter surface with a pore size of 0.2 to 200 μm, separation or sedimentation (sedimentation). Wash the precipitate with distilled water, mainly 1-10 liters of water per 1 kg of sediment. Next, the resulting product is dried birch wax - buttery product is brown in color with a specific smell, which is a complex mixture of fatty, so-called Severinovich acids. To accelerate drying it is carried out at a temperature of 50-125°and a pressure of from 0.01 to 0.10 MPa at paramasivan and crystals. Bast additionally crushed to particles of 0.1-5.0 mm, mix them with water in an amount of 7-10 liters per 1 kg of particles of bast and maintain the resulting mixture at a temperature of 15-40°C for 1-10 days. Next, separate the precipitate from the resulting product - the birch of kvass, the precipitate was separated by filtration or separation. Birch brew is a greenish-yellow liquid, pungent taste, with a characteristic birch odor density of 0.90-1.10 g/cm3and pH 4.0 to 5.5. The precipitate is dried, obtaining the product - feed additive for farm animals and birds.

Example 1. After grinding of birch bark on the crusher and separation of bark and phloem in capacitive extractor volume of 1 m3with anchor stirrer, reflux condenser and a false bottom load 100 kg of crushed bark moisture 1.5% and 500 kg azeotropic mixture of tetrachloroethylene - water, bring the mixture to boil at a temperature of 89°and a pressure of 0.1 MPa and a stand off with a stirrer for 1 hour. After this, the solution is separated from the meal at a temperature of 90°filtered through mickleby filter and placed in a mold with a propeller stirrer volume 0,63 m3, cooled to 25°C and maintained when the mixer 4.5 hours. The precipitated crystals are separated from mother liquor by filtration through calico, washed with distilled water in an amount of 0 l, dried in a shelf dryer at a temperature of 115°and a pressure of 0.05 MPa for 6 hours. Received the product in the amount of 11 kg is a mixture of triterpene compounds, including betulin. Washing fluid is directed into the collection. The mother liquor is evaporated to dryness, add in the apparatus of distilled water in the amount of 100 liters, stirred by the stirrer, separating the solid phase from the washing liquid by filtration through calico, removed from the filter and dried in a shelf dryer at a temperature of 115°and a pressure of 0.05 MPa for 10 hours. The resulting product in an amount of 10 kg is a mixture of triterpene compounds, including betulin. Washing fluid is directed into the collection. Remaining in the extractor meal pour distilled water in the amount of 360 HP Bring the mixture to a boil and maintain the mixture to a temperature of 100°C, after which complete the process of distillation of the solvent from the meal and washing liquid. The collected solvent is collected in a collection and sent for extraction. The meal with water, add sodium hydroxide and hot (55° (C) isopropyl alcohol at the rate of 0.1 kg NaOH and 2 kg of isopropyl alcohol per 1 kg of meal, the mixture is brought to a boil, soak for 3 hours, and then separating the solid phase from the solution by filtration through mickleby iltr, dried in a shelf dryer at a temperature of 110°and the pressure of 0.10 MPa for 5 hours. Received the product in the amount of 35 kg represents the lignin. From the filtrate distilled isopropyl alcohol, the remaining solution was acidified to pH=5.0 with acetic acid. Withstand the acidified solution at a temperature of 15°C for 10 hours under stirring. Next, separate the precipitation from the solution by filtration through mickleby filter. Wash the precipitate on the filter with distilled water. Then dried in a shelf dryer at a temperature of 80°and the pressure of 0.10 MPa for 8 hours. Received the product in the amount of 30 kg is a birch wax. The bast in the amount of 100 kg of additional crushed to particles of 3 mm, mix them with water in an amount of 7 liters per 1 kg of particles of bast and maintain the resulting mixture at a temperature of 30°C for 6 days. Next, separate the precipitate from the resulting product - birch brew filtered through mickleby filter. The precipitate is dried, obtaining the product - feed additive for farm animals and birds in the amount of 80 kg

Example 2. After grinding birch bark and split it into the bark and phloem in capacitive extractor as in example 1, load 50 kg shredded bark moisture 2.5% and 500 kg azeotropic mixture of tetrachloroethylene - water, bring the mixture to a boil, approximately what about 105° C, and incubated with the mixer for 0.5 hours. After this, the solution is separated from the meal at a temperature of 80°filtered through mickleby filter and placed in a mold with a propeller stirrer, cooled to -5°C and maintained when the stirrer for 1 hour. The precipitated crystals are separated from mother liquor by filtration through calico, washed with 20%aqueous solution of alcohol 5,0 l, dried in a shelf dryer at a temperature of 50°and a pressure of 0.01 MPa for 10 hours. The resulting product in an amount of 5 kg is a mixture of triterpene compounds, including betulin. Washing fluid is directed into the collection. The mother liquor is evaporated to dryness, add in the apparatus of distilled water in a 50 l stirred with a stir bar, separating the solid phase from the washing liquid by filtration through calico, removed from the filter and dried in a shelf dryer at a temperature of 125°and a pressure of 0.05 MPa for 5 hours. Received the product in the amount of 4.5 kg is a mixture of triterpene compounds, including betulin. Washing fluid is directed into the collection. Remaining in the extractor meal pour distilled water in an amount of 20 liters Bring the mixture to a boil and maintain the mixture to a temperature of 100°C, after which complete the process of distillation is astorias of the meal and washing liquid. The collected solvent is collected in a collection and sent for extraction. The meal with water, add sodium hydroxide and hot (55° (C) isopropyl alcohol at the rate of 0.15 kg of NaOH and 5.0 kg of isopropyl alcohol per 1 kg of meal, the mixture is brought to a boil, soak in for 5 hours, and then separating the solid phase from the solution by filtration through mickleby filter, dried in a shelf dryer at a temperature of 50°and the pressure of 0.10 MPa for 10 hours. Received the product in the amount of 17 kg represents the lignin. From the filtrate distilled isopropyl alcohol, the remaining solution was acidified to pH=4,5 carbonic acid. Withstand the acidified solution at a temperature of -5°C for 0.5 hour with stirring. Next, separate the precipitation from the solution by filtration through mickleby filter. Wash the precipitate on the filter with distilled water. Then dried in a shelf dryer at a temperature of 80°and the pressure of 0.10 MPa for 10 hours. Received the product in the amount of 15 kg is a birch wax. Bast additionally crushed to particles of 5 mm, mix them with water in an amount of 8 liters per 1 kg of particles of bast and maintain the resulting mixture at a temperature of 15°C for 10 days. Next, separate the precipitate from the resulting product - the birch of the brew. The precipitate is dried, obtaining the product - feed additive for agricultural the state of animals and birds 90 kg

Example 3. After grinding of birch bark on the crusher and separation of bark and phloem in capacitive extractor as in example 1, load 100 kg of crushed bark moisture 2.0% and 200 kg azeotropic mixture of tetrachloroethylene - water, bring the mixture to boil at a temperature of approximately 115°and a pressure of 0.1 MPa and incubated with mixer 1.4 hours. After this, the solution is separated from the meal at a temperature of 100°filtered through mickleby filter and placed into a mold, cooled to 10°C and maintained when the stirrer 5 hours. The precipitated crystals are separated from mother liquor by filtration through calico, washed with distilled water in an amount of 10 l, dried in a shelf dryer at a temperature of 125°and a pressure of 0.05 MPa for 6 hours. Received the product in the amount of 12 kg is a mixture of triterpene compounds, including betulin. Washing fluid is directed into the collection. The mother liquor is evaporated to dryness, add in the apparatus of distilled water in the amount of 11 liters, stirred by the stirrer, separating the solid phase from the washing liquid by filtration through calico, removed from the filter and dried in a shelf dryer at a temperature of 75°and a pressure of 0.1 MPa for 10 hours. Received the product in the amount of 9 kg is a mixture of t is terpenoid compounds, mostly due to betulin. Washing fluid is directed into the collection. Remaining in the extractor meal pour distilled water in the amount of 500 liters Bring the mixture to a boil and maintain the mixture to a temperature of 100°C, after which complete the process of distillation of the solvent from the meal and washing liquid. The collected solvent is collected in a collection and sent for extraction. The meal with water, add sodium hydroxide and hot (50° (C) isopropyl alcohol at the rate of 0.15 kg of NaOH and 5.0 kg of isopropyl alcohol per 1 kg of meal, the mixture is brought to a boil, soak in for 5 hours, and then separating the solid phase from the solution by filtration through mickleby filter, dried under stirring in a dryer at a temperature of 115°and the pressure of 0.10 MPa for 4 hours. The product received 34 kg represents the lignin. From the filtrate distilled isopropyl alcohol, the remaining solution was acidified to pH=5,5 hydrochloric acid. Withstand the acidified solution at a temperature of 25°C for 15 hours under stirring. Next, separate the precipitation from the solution by filtration through mickleby filter. Wash the precipitate on the filter with distilled water. Then dried in a shelf dryer at a temperature of 50°and a pressure of 0.01 MPa for 7 hours. Received the product in the amount of approximately 35 cgrectmake a birch wax. The bast in the amount of 100 kg advanced pulverized to a maximum particle size of 0.1 mm, mix them with water in an amount of 10 liters per 1 kg of particles of bast and maintain the resulting mixture at a temperature of 40°C for 1 day. Next, separate the precipitate through mickleby filter from the received product - birch brew. The precipitate is dried, obtaining the product - feed additive for farm animals and birds - 80 kg

The inventive method provides a comprehensive waste-free processing of birch bark to produce salable products.

1. The method of processing of birch bark, including serial shredding bark in the crusher; the division into the bark and phloem; extraction of birch bark solvent in the form of an azeotropic mixture of tetrachloroethylene - water for 0.5 to 1.4 hours at a temperature of 89-115°C, a pressure of 0.1-1.0 MPa; separating the solution from the meal at a temperature of 80-100°With, keeping the filtrate in the mould for 1-5 hours at a temperature of from -5 to 25°s; separation of precipitated crystals from the mother liquor, washing the crystals with distilled water or 20%aqueous a solution of ethyl alcohol, followed by drying the obtained product is a mixture of three to five triterpene compounds; the process of evaporation of the mother liquor to obtain a dry residue, rinse it with distilled water, followed by drying extracting the aqueous product mix five to seventeen triterpene compounds; removing the solvent from the above-mentioned meal by mixing it with water and subsequent evaporation of the mixture to remove the solvent, mixing the resulting meal with sodium hydroxide and isopropyl alcohol, boiling the mixture for 0.5-5.0 hours, separating the solution from nerastvorimogo precipitate at a temperature of 40-80°With the washing of nerastvorimogo precipitate with distilled water, followed by drying the obtained product lignin; the distillation of the filtrate of isopropyl alcohol, the acidification of the remaining solution to pH 4.5-5.5 and restraint at a temperature of from -5 to 25°C for 0.5 to 15 hours, separating precipitated precipitate from the solution, washing the precipitate with distilled water, followed by drying the obtained product - birch wax; cutting pieces to particles of 0.1-5 mm, mixing them with water in an amount of 7-10 liters per 1 kg of particles of bast, the extract mixture at a temperature of 15-40°C for 1-10 days, separating the precipitate from the resulting product - kvass; drying the precipitate, which is added to animal feed for farm animals and birds.

2. The method according to claim 1, characterized in that the grinding crust is carried out in a knife mill without grates and regrinding in a hammer mill with the holes in the grate.

3. The method according to claim 1, ex is different, however, the separation of the crushed bark on bark and phloem carry on an inclined plane with holes of arbitrary shape, to fit into the circle d 1-15 mm, oscillating in the horizontal and vertical planes with the amplitude of 5-150 mm, a frequency of 1-300 Hz.

4. The method according to claim 1, characterized in that the extraction is carried out at a mass ratio of bark and solvent 1:(2-10).

5. The method according to claim 1, characterized in that the above extraction was carried out with stirring bark and solvent.

6. The method according to claim 1, characterized in that the separation of the precipitated crystals from the mother liquor is performed by filtering through a filter with a pore size of from 0.2 to 200 microns.

7. The method according to claim 1, characterized in that the washing of the crystals with distilled water or 20%aqueous solution of ethanol is carried out in a volume of 1-10 liters per 1 kg of crystals.

8. The method according to claim 1, characterized in that the drying of the obtained product is a mixture of 3-5 triterpene compounds is carried out at a temperature of 50-125°and a pressure of from 0.01 to 0.10 MPa.

9. The method according to claim 1, characterized in that the drying of the obtained product is a mixture of 3-5 triterpene compounds are under stirring of the product.

10. The method according to claim 1, characterized in that the washing referred to the dry residue distilled water is carried out in a volume of 1-10 liters of water per 1 kg of dry residue.

11. With whom persons according to claim 1, characterized in that the drying of the obtained product is a mixture 5-17 triterpene compounds is carried out at a temperature 50-125°and a pressure of from 0.01 to 0.10 MPa.

12. The method according to claim 1, characterized in that the drying of the obtained product is a mixture 5-17 triterpene compounds are under stirring of the product.

13. The method according to claim 1, characterized in that the said meal is mixed with water in the ratio 1:(1-10) parts by weight of

14. The method according to claim 1, characterized in that the dry meal is mixed with sodium hydroxide and isopropyl alcohol in the following ratio of components: sodium hydroxide - 0,10-0,15 kg; isopropyl alcohol - 2,0-5,0 kg per 1 kg of dry meal.

15. The method according to claim 1, characterized in that the separation of the solution from nerastvorimogo in sodium hydroxide and isopropyl alcohol precipitate is carried out by filtering through a filter with a pore size of from 0.2 to 200 microns.

16. The method according to claim 1, characterized in that the washing of nerastvorimogo in sodium hydroxide and isopropyl alcohol precipitate with distilled water is carried out in a volume of 1-10 liters of water per 1 kg of sediment.

17. The method according to claim 1, characterized in that the drying of the obtained product of lignin is carried out at a temperature of 50-125°and a pressure of from 0.01 to 0.10 MPa.

18. The method according to claim 1, characterized in that the drying of the obtained product of lignin is carried out at a stirring of the product.

19. The method according to claim 1, characterized in that popcicle is their solution, remaining after the distillation of the filtrate isopropyl alcohol, lead acetic acid.

20. The method according to claim 1, characterized in that the acidification of the solution remaining after the distillation of the filtrate isopropyl alcohol, lead hydrochloric acid.

21. The method according to claim 1, characterized in that the acidification of the solution remaining after the distillation of the filtrate isopropyl alcohol, lead carbonic acid.

22. The method according to claim 1, characterized in that the branch fell from the acidified solution precipitate is carried out by filtering through a filter with a pore size of from 0.2 to 200 microns.

23. The method according to claim 1, characterized in that the rinsing dropped out of the acidified solution of the precipitate with distilled water is carried out in a volume of 1-10 liters of water per 1 kg of dry residue.

24. The method according to claim 1, characterized in that the drying of the resulting product - the birch of the wax is carried out at a temperature 50-125°and a pressure of from 0.01 to 0.10 MPa.



 

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