The method of obtaining betulin

 

(57) Abstract:

The invention relates to extraction of valuable chemicals from waste timber, namely the allocation method betulin formula I from birch bark. Describes the method of obtaining betulin from birch bark, including its activation at a temperature of 180-260oC, a pressure of 2-5 MPa for 50-300, the treatment with alkali and extraction of alcohol, according to the invention the activation of birch bark and its alkaline hydrolysis is carried out simultaneously with the alkali charge in the amount of 10-20% by weight of the absolutely dry bark. The technical result of the invention is to reduce the duration of the process, as well as reducing consumption of alkali at the stage of hydrolysis. 1 PL.

The invention relates to extraction of valuable chemicals from waste timber, namely the allocation method betulin formula I from birch bark birch

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Betulin - white crystalline powder, So pl.= 261 - 262oC, practically insoluble in water, soluble in alcohol. Betulin is non-toxic, used in medical, cosmetic and chemical industries [1].

A method of obtaining betulin, implying ">

Shredding bark in an aqueous alkali solution is complex in terms of technology, as is done mechanically and therefore requires high energy costs. In addition, the disadvantage of this method is the duration of the extraction operation and consequently, the low efficiency of the process.

The closest technological essence and the achieved result is a method of obtaining betulin from birch bark, including preliminary activating it in pisabarro of paratrechina at a temperature of 180 260oC, pressure of 2 to 5 MPa for 60-360 sec and subsequent extraction in aqueous alcoholic alkaline environment [3].

This method is characterized by insufficient intensity extraction of betulin from birch bark in the conditions pisabarro of paratrechina at a temperature of 180 260oC, a pressure of 2 to 5 MPa for 60 to 360 seconds, due to weak hydrolysis in linopetra complex. Basically at the moment of the abrupt pressure release is loosening the bark in the dust. For the complete extraction of betulin is necessary to have a stage - exhaustive hydrolysis limnogeology complex shredded bark using a big calicification the extraction of betulin, simplification of the production technology by combining the stages of activation of birch bark and its alkaline hydrolysis. The technical result of the invention is to reduce the duration of the process, as well as reducing consumption of alkali by hydrolysis step.

The problem is solved in that in the method of obtaining betulin from birch bark, including its activation at a temperature of 180-260oC, a pressure of 2-5 MPa for 60 to 300 seconds, the treatment with alkali and extraction of alcohol, according to the invention the activation of birch bark and its alkaline hydrolysis is carried out simultaneously with the alkali charge in the amount of 10 - 20% by weight of absolutely dry bark.

Comparative analysis with the prototype shows that the distinctive features of the prototype feature is the activation of birch bark simultaneously with alkaline hydrolysis, the amount of alkali charge within the specified limits.

Conducting hydrolysis of birch bark together with its activation conditions pisabarro of paratrechina, i.e., at a temperature of 180-260oC, a pressure of 2 to 5 MPa for 60 to 360 seconds, allows you to conduct an exhaustive hydrolysis limnogeology complex of birch bark, which improves the intensity of extraction of betulin. In addition to that is araraquara, because the high temperature and pressure cause extensive hydrolysis limnogeology complex bark and at low alkali concentration. Thanks to the combination of the stages of activation and alkaline hydrolysis reduces the duration of extraction of betulin, because there is no separate stage of processing lye.

The process is as follows. Technological bark previously subjected to activation conditions pisabarro of paratrechina in the presence of alkali, taken in an amount of 5 to 20% by weight of the absolutely dry bark. Naysabury precracking performed at a pressure of 2 to 5 MPa, a temperature of 180 260oC, activation time of 60 to 300 sec. When conducting pisabarro of paratrechina (activation) in the presence of alkali is very rapid hydrolysis of birch bark, and when a sudden pressure relief remains non-hydrolyzed material (bark) razryhlyaya in the dust.

The bark of the birch after conducting pisabarro of paratrechina in the presence of alkali is a smooth, creamy mass of gray.

The hydrolysate bark (after activation in the presence of alkali) diluted with alcohol and boil for 2 to 5 minutes, separate the alcohol solution of Betuline 1. 100 g of bark humidity 5% with the content of betulin 35% is loaded into the reactor, heated to a temperature of 240oC. and Then poured on 30 ml of an aqueous solution containing 20 g of NaOH. Within 2 to 3 seconds with saturated steam pressure increases to 3.4 MPa and incubated for 240 sec. Then using a ball valve provide a sharp pressure relief, while the hydrolyzed material is dropped into the receiving tank. The hydrolysate is homogeneous gray mass. The hydrolysate is transferred into the reactor or flask with reflux condenser, pour 2 liters of ethyl alcohol and brought to a boil. Hot alcohol solution is separated by filtration, distilled alcohol. Fallen betulin is filtered off, washed on the filter with hot water, dried. Exit 34% by weight of the absolutely dry bark (extraction rate 97%).

In the table (see below) shows the output of betulin, in parentheses, the degree of extraction in % depending on the NaOH concentration and the time of activation conditions pisabarro of paratrechina by extraction with ethyl alcohol.

As can be seen from the table, the maximum yield of betulin is achieved when the alkali concentration of 10 - 20%. When the alkali concentration below 10% hydrolysis of birch bark passes slightly, due to the substantial increase in the yield of betulin, in addition, quality is deteriorated due to the secondary processes of destruction.

The proposed method allows to intensify the process of obtaining betulin. First proposed to activate the bark of the birch in the process of conducting pisabarro of paratrechina in the presence of alkali, which allowed us to exclude, as an independent stage of hydrolysis of birch bark, because simultaneously with the activation of birch bark neishaburi paratrechina in the presence of alkali is and its complete hydrolysis. However, more than 30 times reduces the amount of alkali used, so, in prototype 3 g activated birch bark is taken 20 g NaOH, and the proposed method on 100 g of birch bark to 10 to 20 g NaOH.

Optimal conditions for pisabarro of paratrechina: pressure of 3.4 MPa, temperature 240oC, the amount of alkali 10 to 20% by weight of the bark, the activation time depending on the size of wood chips bark and the concentration and type of alkali (NaOH or KOH) can vary from 60 to 300 sec.

Literature

1. Jaaskelainen P. Papari ja Puu., 1981, N 10, p.599.

2. USSR author's certificate N 382675, class C 07 J 53/00, 1973.

3. RF patent N 2074867, class C 08 H 5/04, C 07 J 53/00, 63/00.

FPIC Is P>oC, a pressure of 2 to 5 MPa for 60 - 300, the treatment with alkali and extraction of the alcohol, characterized in that the activation of birch bark and its alkaline hydrolysis is carried out simultaneously with the alkali charge in the amount of 10 - 20% by weight of absolutely dry bark.

 

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11 cl, 1 tbl, 9 ex

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