Vegetable oil-based product manufacture method
FIELD: food industry.
SUBSTANCE: composition is concentrated in terms of compound ethers of pinosylvine and produced by way of crude tall oil distillation or evaporation; the compound ethers acidic residue is formed by linoleic, linolenic, oleic acid or tricyclic, aliphatic or aromatic carboxylic acid. Stilbenes are extracted from the crude tall oil distillation or evaporation fraction containing stilbenes compound ethers; the fraction is concentrated. Then the stilbenes compound ethers are modified into the desired stilbenes by way of stilbenes compound ethers separation from their compound ether group. The crude tall oil distillation or evaporation fractions contain pinosylvine or its compound ethers in an amount of 5 - 95 % of the total weight of the composition.
EFFECT: invention relates to fat-and-oil industry, in particular, to a composition suitable for stilbenes production, to its production method, to a method for extraction of stilbenes from crude tall oil, to a compound ether of resin acid and pinosylvine or to its simple monomethyl ether.
26 cl, 1 dwg, 3 ex
The invention relates to compositions according to the preamble to claim 1.
The invention relates to a method of making a composition suitable for obtaining stilbene according to the preamble of item 13.
In addition, the invention relates to a process for the preparation of stilbene and its derivatives from compounds containing penicillin or its derivatives.
Tall oil typically contains a stilbene. Examples of the stilbene include, among others, TRANS - and CIS-stilbene, resveratrol, piceatannol and pinosylvin. Typically, these compounds contain two benzene rings connected by an ethylene chain, while the last three of these compounds are hydroxy-substituents in one or both of the benzene rings.
The formation of these compounds occurs in the wood during the normal growth of the tree. Upon receipt of the pulp by the sulphate process is contained in the wood stilbene at least partially transformed into a by-product, namely the flow of crude tall oil. In the analysis of literature data, it was found that the number (%) of stilbene in the composition of the crude tall oil is too insignificant to consider their separation and isolation from the above source as a cost-effective process.
Therefore, the present invention is to develo the TKA allocation method of stilbene, in particular pinosylvin and its derivatives from crude tall oil (hereinafter STM) and of the products obtained by evaporation and distillation specified tall oil. Another objective of the present invention is to provide compositions containing esters pinosylvin and simple nanometrology ether pinosylvin, and methods for obtaining such compounds.
The present invention is based on the discovery that the stilbene, in particular derivatives pinosylvin, go into different factions products in the distillation process of tall oil, depending on their molecular weight and boiling abilities. During the distillation STM under certain conditions pinosylvin and its simple onomatology ether form, inter alia, esters of fatty and resin acids, resulting in their molecular weight generally increases. In this case there is the possibility of their separation from the main streams of distillates, which include fatty acids and/or rosin acid.
Unexpectedly it was discovered that these compounds are concentrated in those distillation fractions, which were not considered for further processing and to date has been removed and burned or used as salvage. In the framework of the present invention, it was found that the defined fractions contain, in contrast to what was previously known, so a significant number of these stilbene, after concentration, they form the most preferred feedstock to obtain stilbene.
More specifically, the compositions according to the present invention described in the characterizing part of claim 1.
In turn, the method according to the present invention described in the characterizing part of item 13.
In turn, the compounds according to the present invention is characterized in distinctive parts p and 34.
The present invention allows to achieve a number of significant advantages. So, through the process has become possible to select from tall oil in industrial scales brand-new valuable products and groups of products, which until now were not available in the commodities market. Derivatives pinosylvin allocated thus, can be used by themselves or for further modification by a variety of chemical methods.
Recent studies show that the stilbene potential for use as food additives that affect the health, or even medicines. According to the present invention have the structure that represents a suitable raw material for production of stilbene, which contains, for example, esters simple nanometrology ether pinosylvin and fatty acids or resin acids. Of these compounds can be obtained, in addition to the specified simple monomethylamine ether pinosylvin, many other stilbene, such as pinosylvin, piceatannol, resveratrol, rhapontigenin and pterostilbene.
In the present invention under the stilbene should understand the above compounds along with their derivatives.
Hereinafter the present invention will be described in more detail with the help of detailed description and the accompanying drawings. The Figure 1 shows a typical block diagram of the distillation of tall oil.
As indicated above, the present invention is based on the discovery that the fractions obtained by distillation or evaporation of tall oil, including waste products of distillation columns and evaporative devices contain an unexpectedly large number of stilbene and their esters, which consequently ensures the suitability of these fractions to highlight these connections.
In the present invention "tall oil is a by-product in the process of obtaining cellulose containing extracts of wood used for cooking pulp.
The main components of tall oil are fatty, resin acids and neutral compounds. Fatty is acid, as a rule, represent unbranched saturated carboxylic acids containing 16 to 24 carbon atoms or carboxylic acid containing 1-3 double bonds. Industrial and commercially important are fatty acids With 18, form the basis of the fatty acids of tall oil. Similarly, resin acids of tall oil are carboxylic acids, but their basic structure is formed by three rings. In tall oil contains several types of resin acids, which differ from each other mainly by the presence of different lateral substituents, as well as the number and position
Derivatives pinosylvin can be in the tall oil in the form of individual compounds, for example, such as pinosylvin (PS), a simple onomatology ether pinosylvin (pmap) and simple dimethyl ether pinosylvin (PDAP).
The Figure 1 shows a typical block diagram of the distillation of tall oil.
As shown in Figure 1, STM through a series of preliminary stages, before it becomes possible separation and resin and fatty acids contained therein.
Due to the low vapor pressure of the feedstock distillation of tall oil is carried out under reduced pressure. In addition, at elevated temperatures, there is a possibility of decomposition of the raw material with the formation of bespoke the different products and, therefore, should strive to maintain a more moderate conditions. Typically, in Europe, people use the "dry method" distillation of tall oil at working pressure of 3-30 mbar. In other countries usually use the "wet method", i.e. the distillation with steam at an operating pressure of about 250 mbar.
Typically, the vacuum in the system is achieved through a series of sequentially connected steam generator or ejectors and liquid ring pumps. The vacuum required in the first stage of acceleration - drying tall oil, should be somewhat less than in the process of acceleration, and is usually achieved by using a liquid ring pump.
Used with pulp production STM contains about 2% water. In the dry method of this amount of water is detrimental to the vacuum device. Therefore, in the first stage, the necessary drying STM, after which are separated from each other by water from the original oil contained in the upper layer of the product. Drying can be carried out, for example, to the separation of the resin by filing a CTM in thin-film evaporator, in which the working pressure is about 40 mbar and a temperature of 200-240°C.
At the stage of drying is the removal of water, turpentine and other volatile components of the STM in the form of product evaporation. The product is condensed before on stagnet vacuum installation and in most cases, mixed with oil flow coming from the ejector. After drying STM immediately sent to obessmolivajushchie installation, typically formed from two series-connected thin-film evaporators or columns to separate the resin. The task at this stage is more thorough separation of volatile compounds from STM volatile ingredients. Volatile compounds out of the evaporator in the form of a gaseous product and directly forwarded either directly in the form of gas, either through evaporation of liquid in the column for separation of resin acids.
In addition to the gas stream exiting the vacuum unit, as a rule, also formed of a mixture of water and light organic compounds, organic and aqueous phase which is usually separated from each other by gravitational desantirovaniya. The organic phase better known as the ejected oil usually contains turpentine, and very volatile acids and neutral compounds included in the PL.
From STM is formed approximately 2-4% of the ejected oil. Water is removed by decantation, contains in addition to moisture or condensed steam used by vacuum as a means for their work, and also the water contained in the wet STM, fewer than 2% of the number of STM. Ejected the e oil is mainly used as a fuel oil heating boilers distillation.
When distillation of the Northern varieties STM amount of discharge of the resin is 30% of the dried STM. The majority of the allocated resin is used as biofuel. The resin contains about 10-15% of sitosterol, either in pure form or in the form of esters. This leads to the fact that many companies in the world produce sitosterol from resins for sale for further use as food additives in food products that affect health.
Distilled fraction separated resin is sent to the column for separation of resin acids, distillation products emit resin acids, and as a product of the upper layer of lighter fractions. Next, from the remainder of the original oil is separated mainly in the first column and the second fatty acid. Fatty acids are usually isolated in the form of a fraction in the second column, in which the VAT of the product is base oil. In addition to resin acids and heavy fatty acids, formed during earlier stages of the distillation, at the bottom of the column to separate the fatty acid concentrate other volatile ingredients components distillation. This thread combine directly with a resin and, as a consequence, ultimately, used as biofuel for energy production. Products VAT residue column for separating oily to the slot together account for 4-6% of STM. The problem lies in the concentration of 18 fatty acids, forming part of tall oil, the fraction containing fatty acids described above. When distillation of the Northern varieties of tall oil output fatty acids 35-40% of the number of input dry STM. Usually fatty acids are used in the production of alkido, i.e. binders for paints, by obtaining esters based on fatty acids and certain polyalcohol.
Resin acids are concentrated in products of resin acids, which are in the processing of the Northern varieties STM is about 22-25% based on dry STM. Resin acids using, for example, in the production of esters and adhesives.
In a distillation apparatus with a low dividing ability to allocate enough pure resin and fatty acids, there is a need to take the product fraction is called distillirovannoi tall oil. This fraction mainly contains fatty acids, and 25-35% resin acids and a small amount of neutral substances. The heavy fraction and consequently the most volatile ingredients is tall oil resin. Short-chain (usually 16) fatty acids and volatile neutral substances are concentrated in the original tall oil. Typically, the original is the material oil is selected at the top of each distillation column, but in the most advanced distillation process - only on special column for initial selection of tall oil. In the Northern varieties of the content of the original tall oil is 7% of the number of dry STM. To date, further processing for the original tall oil does not exist and, as a consequence, this oil is mainly used as a natural renewable fuels.
In both variants of the basic process, the temperature of the columns in the upper part is typically in the range of 160-180°C., and the temperature of the cube 240-275°C. The high-temperature stage distillation is carried out by separation of the resin, the temperature is usually 300-320°C.
When using columns to separate the resin in the separation of the resin volatile substances are selected in the upper part of the column, for further acceleration, and the resin forms VAT residue.
VAT product obtained in the process of separating resin is a resin of tall oil. At least distillation residues from the primary distillation process, containing a large amount of high-boiling substances, as well as measurable selection of resin acids, usually return to the stage of separation of the resin. Conditions stage of separation of the resin are 30 mbar and 300-320°C.
The flow of gas and/or liquid, based on their from the stage of separation of the resin, refer to the column for separation of resin acids. This column usually is the selection of four factions: the top of the column are likely to be selected initial tallowa oil; below is a crude fraction of fatty acids, which is then channelled to the column for separation of the original tall oil; from the lower part of the column is the selection of a gaseous fraction of resin acids for instant condensation; with the bottom of the boiler have a feedback thread for the Department of the resin. In addition, under the former processes the pickup selection distilled tall oil (ATT) was made from a point located just above the sampling point fraction of resin acids. In addition, the sampling fraction of resin acids was carried out in the lower part of the column or the bottom of the boiler.
Column for separation of the resin acids are usually filled with nozzle plates, specially made for vacuum distillation, the lower the boiler of the column is a falling film evaporator or evaporator with forced circulation. Other columns - a column for separating the original tall oil and the column for the separation of fatty acids in the typical process of acceleration of tall oil has a similar structure columns for separation of resin acids. The raw composition of fatty acids, warded off from the column to separate malenich acids, refer to the column for separation of the original tall oil. Usually from the column there are two streams of products: original oil on top, and the stream known as the crude fatty acids from below.
Careful separation of the original tall oil is material if there is a need for svetoustojchivyh and as light chain fatty acids. Distillation of the products from the column to separate the original tall oil is directed to the column for separation of fatty acids, where the separation of three fractions: again with the upper part of the column is the original tall oil sent further back in the column for separating the original tall oil, a little lower fatty acids, and from the bottom of the boiler, the so - called kubovo oil.
In the framework of the present invention, it was found that during the refining of crude tall oil by the above process, the pickup tall oil is the distribution of stilbene in different fractions of the products of distillation. At various stages of separation and storage there is a possibility of interaction between PS and pmap with the basic components of tall oil, in particular of fatty and resin acids with the formation with the above fatty acids and resin acids esters pinosylvin or simple m is nematologia ether.
Behavior esters pinosylvin and simple monometallic esters by distillation of tall oil is significantly different from the corresponding behavior of acids or derivatives pinosylvin. These esters are high-boiling compounds, so they go in distillation fraction products the pickup, while the available connections pinosylvin and fatty acids and resin acids pass into the other factions products by distillation.
In the framework of the present invention it was also found that the esterified stilbene adversely affect the quality of the products the pickup tall oil, causing a darkening of the color of the distillate. Therefore is the preferred them to be more careful separation from the main products of the distillation, namely from the fatty and resin acids.
There is the possibility of separating unreacted stilbene from the lungs distilled fractions of tall oil, while the stilbene, esterified with fatty acids and/or rosin acids, or stilbene, which came in other reactions and, thus, become less volatile, can only be allocated from the distillation fractions of the products of distillation.
When the esters of derivatives of stilbene, which acid residue formed acid with low m the molecular mass, there is the possibility to transfer the formed esters also in the light fractions.
In addition, it should be noted that there is a possibility of separation of the stilbene compounds from caught in the vacuum distillation, in that case, if using steam distillation process for the distillation of tall oil.
According to the present invention have the composition, suitable for receiving stilbene containing pinosylvin derived pinosylvin, ester pinosylvin or ester derivative pinosylvin, or mixtures of these compounds. The most suitable are concentrated formulations, i.e. the compositions, enriched with respect to these compounds. The "concentration" includes, among other things, an option in which other components are removed from the composition containing the derivatives of stilbene, while the percentage of derivatives of stilbene increases, the option of the composition is separated and isolated in pure form derivatives of stilbene.
In accordance with one preferred implementation, the composition contains esters simple nanometrology ether pinosylvin, acid residue which is formed of an organic or inorganic acid, in particular an organic acid present in the crude tall oil or the image is in my process. Typically, these acids are fatty acids, resin acids and lower alcamovia acid.
Therefore, an acid residue of esters can be formed carboxylic acid with unbranched hydrocarbon chain containing 16-24 carbon atoms or a fully saturated or comprising 1-3 double bonds. More preferably, the acid residue of ester simple nanometrology ether pinosylvin formed linoleic acid, linolenic acid or oleic acid.
It is also possible, when acid residue esters pinosylvin or simple nanometrology ether pinosylvin formed tricyclic, aliphatic or aromatic carboxylic acid. Examples of such acids include abietic acid, dehydroabietic acid, neoabietic acid, Polustrovo acid, pimaric acid, and levopimaric acid.
When this acid residues of esters can be formed by a single acid or a mixture of two or more acids.
In General derived pinosylvin form about 0.1-20 wt.% from distillation fractions of the product, subject to Department, but you can concentrate this composition by separating lighter components, for example, by evaporation. After this stage of separation of the contents of stilbene with the hat at least 3 wt.%, preferably about 5-80 wt.%, more preferably about 5-50 wt.% by weight of the total composition.
Share pinosylvin, esters pinosylvin, simple nanometrology ether pinosylvin, esters simple nanometrology ether pinosylvin or simply dimethyl ether pinosylvin, or a mixture of two or more compounds contained in the composition is about 1-95 wt.%, preferably about 10-60 wt.%, more preferably about 15-50 wt.% by weight of the total composition.
Thus, in accordance with one variant of implementation of the composition according to the present invention contains a resin, tall oil, concentrated to increase the proportion of esters in stilbene.
In the method according to the present invention the fraction containing esters of stilbene, isolated from the fractions obtained by distillation or evaporation of the crude tall oil, and further enrich towards it contains esters of stilbene, after which the esters of stilbene change in the desired stilbene by separating esters of stilbene from their ester groups. Preferably, these fractions obtained by distillation or evaporation, was a fraction of the products of the upper layer, distillation products or fractions taken from the side through the selected outlet of distillation Colo is able or evaporator, or stream directed into the vacuum system.
Esterified the stilbene during the process of acceleration of tall oil predominantly pass into the resin, and, in particular, distillation products columns for the separation of fatty acids.
Therefore, in accordance with one variant of the invention the fractions containing esters of stilbene, isolated in the form of a bottom fraction columns for the separation of fatty acids.
In addition, you can also select a mixture containing a stilbene or their esters, in the form of products of the upper layer by distillation or evaporation of tall oil, but in fact is possible only as the products of the upper layer in the column for separating light of fatty acids. The stilbene forming part of the products of the upper layer, if necessary, accelerate their concentration, can be tarifitsirovana, but not necessarily. As tarifitsiruemih acid can be used both organic and inorganic acids. Examples of such acids include lower alcamovia acids, resin acids and fatty acids.
After the esterification of the stilbene concentrate in relation to the product of the upper layer, and the separation can be carried out without any esterification using well-known chemical engineering separation techniques.
Threads formed in the process is Ashanti tall oil, can be combined to obtain a suitable raw material. Accordingly, the composition that is particularly suitable for stilbene, is obtained by combining distillation fractions of the column for the separation of fatty acids and products of the upper layer of the column to separate the lungs fatty acids.
Simply concentrate stilbene by evaporation at low pressure distillation products columns for the separation of fatty acids, as well as from other threads, formed by the distillation of tall oil. The process of evaporation can be carried out in the evaporator with forced circulation, falling film evaporator, thin film evaporator or evaporator with a small distance from the heater to the condenser, or other devices suitable for evaporation under low pressure. Alternative separation methods include inter alia repeated distillation, extraction, chromatographic separation, ion-exchange methods, adsorption, absorption, vacuum distillation and separation crystallization. In addition, when the concentration of the compounds can be applied to various filtration methods, such as filtration using membranes.
The above methods of separation can also be applied when esters pinosylvin to destroy the separation or by pre the treatment of esters in the original products, or other derivatives of these original products. Reaction that destroys esters, can be carried out either in aqueous medium or in the medium of solvent and using, if necessary, auxiliary substances, which provide alkaline conditions, or other reagents that facilitate the destruction of esters.
Another method of separation is a transesterification, in which the alcohol residue of ester, in particular pinosylvin, replaced by another alcohol.
It was found that during normal acceleration tall oil derivatives pinosylvin form esters with fatty and resin acids. Due to the fact that these esters can be separated from other products of the distillation of tall oil is much easier than derivatives pinosylvin in its pure form, it is possible to accelerate the formation of esters by treating mixtures subject to distillation, additives that catalyze the esterification at different stages of the process, for example, acids or compounds capable of generating hydrogen ions (protons) in collaboration with fatty or rosin acids. It is known that hydrogen ions (protons)in a mixture of acid, or released in the course of different reactions catalyze the esterification reaction. As catalyzing the process of esterification EXT the file, you can use the oxygen.
Of the compounds according to the present invention, the stilbene isolated in the form of esters of various acids, in particular mineral or alkanovykh acids, fatty acids, resin acids, and mixtures thereof.
Department of stilbene-free fractions, it is possible to implement the same techniques that were described above in respect of their esters. The stilbene can also be modified using other methods of chemical technology, for the formation of compounds that are easier to separate from the rest of the factions than the original. Accordingly, the stilbene contained in the products of distillation, may be susceptible to interaction with the formation of esters or salts to accelerate their further separation. The classical method of separation of phenolic compounds, which often include derivatives pinosylvin, from carboxylic acids is the treatment of the mixture with sodium bicarbonate, which resulted in the acid form salts, and phenolic compounds no.
The present invention may find application in obtaining pinosylvin, piceatannol, rhapontigenin, resveratrol or pterostilbene or any other derivatives of stilbene, having one or more hydroxyl and/or ether groups, or any other derivative of the above stilbene.
The following neogenic the living examples illustrate the present invention:
Raw fatty acids, resulting from the acceleration of tall oil, evaporated in the evaporator with a small distance from the heater to the condenser at a pressure of 5 mbar and a temperature of 220-240°C. In a stream of distillate was 85-97% of the total flow, and the flow distillation products, respectively 3-15%.
The results GCMS (gas chromatography-mass spectrometry) analysis of the distillation product of the contents of esters simple nanometrology ether pinosylvin was 3-30 wt.% together with fatty acids or resin acids.
Earlier analysis had not revealed either to demonstrate the presence of these substances.
CBM product experiences described above were processed within four hours and 15 wt.% with a mixture of water and solid alkali (NaOH) while heating and stirring. Then the aqueous phase was separated from the organic. The organic phase is again evaporated in the evaporator with a small distance from the heater to the condenser at 5 mbar and 160-270°C.
In the resulting distillate content simple nanometrology ether pinosylvin varied in the range of 25-60 wt.%.
In another process, the concentration of CBM product obtained in Example 1 in the distillation of crude fatty acids are first processed by heating and stirring 15 mass. with a mixture of water and solid alkali to destroy esters in the solution of free alcohols and salts of acids.
Further added 30 wt.% sulfuric acid in the organic phase. The reaction mixture is defended, separated aqueous phase from the organic. The organic phase was placed in an evaporator with a small distance from the heater to the condenser (5 mbar, 160-270°C), with the resulting flow of distillate contained 25-60 wt.% simple nanometrology ether pinosylvin.
It should be noted that the volatility of ester simple nanometrology ether pinosylvin different from the volatility of fatty or resin acids so that you can use a traditional vacuum distilled to further purify the simple nanometrology ether pinosylvin through his concentration.
1. A composition, suitable for receiving stilbene, characterized by the fact that he concentrated towards esters pinosylvin and obtained by distillation or evaporation of crude tall oil, and the acid residue of esters formed linoleic, linolenic, oleic acid or tricyclic, aliphatic or aromatic carboxylic acid.
2. The composition according to claim 1, characterized in that the percentage of ester pinosylvin in the composition is at least about 3 wt.%, for example, about 3-80 wt.%, preferably about 5-50 wt.% by weight of the total composition.
3. The composition according to claim 1, characterized in that the acid OS is atok formed abietic, dehydroabietylamine, neoabietic, Polustrovo, pieroway or levopimaric acid.
4. The composition according to any one of paragraphs. 1-3, characterized in that the concentration of dry matter pinosylvin or derivatives pinosylvin is about 3-50 wt.%.
5. The composition according to any one of claims 1 to 3, characterized in that the concentration of ester pinosylvin is about 5-95 wt.%, more preferably about 10-60 wt.%, more preferably about 15-50 wt.% by weight of the total composition.
6. The composition according to any one of claims 1 to 3, characterized in that it contains a fraction distillation or evaporation of crude tall oil, while this fraction was concentrated to increase the share pinosylvin or esters of its derivatives.
7. The composition according to any one of claims 1 to 3, characterized in that it contains a resin, tall oil, which was concentrated with the aim of increasing the share pinosylvin or esters of its derivatives.
8. The composition according to any one of claims 1 to 3, characterized in that the proportion of esters pinosylvin is about 1-95 wt.%, preferably 10-60 wt.%, more preferably about 15-50 wt.% by weight of the total composition.
9. A method of obtaining a composition according to claim 1, suitable for receiving pinosylvin and its derivatives, characterized in that from the fraction distillation or evaporation of crude tall oils extracted fraction which contains esters pinosylvin or its derivatives, next, the concentrate fraction in relation to esters pinosylvin or its derivatives.
10. The method according to claim 9, characterized in that the feed stream to the distillation or evaporation is a fraction, which is the product of the upper layer, kubovy product or intermediate product, taken from the side through the selected hole distillation column or evaporator distillation device of tall oil.
11. The method according to PP-10, characterized in that the fraction containing esters pinosylvin or its derivatives, isolated in the form of a bottom fraction of the distillation column for fatty acids.
12. The method according to PP-10, characterized in that the fraction containing esters pinosylvin or its derivatives, is a tall oil resin.
13. The method according to PP-10, characterized in that the fraction containing esters pinosylvin or its derivatives, isolated in the form of the product of the upper layer of the column or evaporator used in the distillation of tall oil.
14. The method according to item 13, wherein the stilbene forming part of the products of the upper layer, atrificial with lower alkhanovym acids, or fatty acids or resin acids, or a stilbene modify using known chemical methods of obtaining compounds that are more easily separated totalno part of the faction, than the original compound.
15. The method according to 14, characterized in that any product of the upper layer distillation device for tall oil or another product flow concentrate in relation to the stilbene or a derivative after the esterification of the above derivatives.
16. The method according to any of PP-10, 14-15, characterized in that the composition is suitable for receiving stilbene, is formed by combining a bottom fraction of the column for distillation of fatty acids and the product of the upper layer of the column containing light fatty acids.
17. The method according to any of PP-10, 14-15, characterized in that in order to increase the yield of esters of stilbene, crude tall oil or one of its distillation fractions are subjected to conditions conducive to the formation of esters by the reaction between pinosylvin or simple methyl ether pinosylvin and fatty acids or resin acids.
18. The method according to 17, characterized in that the crude tall oil or distillation fraction is brought into contact with the additive that catalyzes the process of esterification.
19. The method according to p, characterized in that as catalyzing the process of esterification supplements use oxygen.
20. The method according to p or 19, characterized in that the connection that produce hydrogen ions in the reaction with the fatty acid or resin KIS the Auteuil used as an additive, catalyzing the process of esterification.
21. The method of selection of stilbene from crude tall oil, characterized in that from the fraction distillation or evaporation of crude tall oils extracted fraction containing esters of stilbene fraction concentrate, after which the esters of stilbene change in the desired stilbene by separating esters of stilbene from their ester groups.
22. The method according to item 21, wherein the stilbene isolated in the form of esters, or mixtures thereof, the lower alkanovykh acids, fatty acids or resin acids.
23. The method according to item 22, wherein the receive pinosylvin, piceatannol, rhapontigenin, resveratrol or pterostilbene or other derivative of stilbene containing one or more hydroxyl and/or ether groups, or any other derivative of these stilinovich connections.
24. Ester resin acids and pinosylvin or simple nanometrology ether.
25. Ester according to paragraph 24, wherein the acid residue formed or tricyclic aromatic carboxylic acid.
26. Ester in paragraph 24 or 25, characterized in that the acid residue formed abietic acid, dehydroabietic acid, neoabietic acid, Polustrovo acid, pieroway acid or levopimaric the acid.
SUBSTANCE: first, sulphate soap is combined with an alkaline washing solution, which has a lower concentration of lignates and inorganic solid substances than the sulphate soap. Resulting mixture includes washed tall oil soap, a concentrated salt solution, lignates and calcium carbonate. After that, washed tall oil soap is separated from the concentrated salt solution, lignates and calcium carbonates, preferably with an application of centrifugation, decantation, filtration, settling or combination of the said technologies. Acidification of washed tall oil soap forms a mixture of crude tall oil and spent acid. Crude tall oil is separated from spent acid. Spent acid is converted into alkali, and, at least, a part of it is returned for a application as alkaline washing solution.
EFFECT: invention makes it possible to manufacture crude tall oil, simultaneously preventing technological shortcomings, caused by the accumulation of calcium sulphate in acidification installations or after them.
18 cl, 13 dwg, 6 tbl, 4 ex
FIELD: machine building.
SUBSTANCE: proposed line comprises stock intake container with coarse filter at its outlet and pump communicated via pipelines, sequentially mounted strainer, centrifuge, separator, finished product collection tank and fat catch basin. Both stock intake container and finished product collection tank are connected with steam generator boiler and equipped with steam control valves and accessories to heat and maintain water-fat emulsion temperature of 90-95°C, steam jacket. Note that said line includes three stock intake containers and three finished product collection tanks equipped with mixers. Aforesaid container is composed of three-phase decanter. Said fat catch basin comprises reinforced concrete parallelepiped-shaped body with inclined bottom and vertical walls atop which detachable false deck is mounted to be removed in removal of supernatant mass layer. Detachable lower false deck is arranged under said upper false deck at distance of at least 30 cm there under to allow routine services or elimination of emergent conditions brought about by shock outbursts. Box adjoins one of vertical walls for fat catch basin reconditioning by hot water or steam, or mechanically in case pipeline to discharge effluents if sewerage is clogged. Effluents feed pipeline is arranged opposite said box on vertical wall. Intake hole for discharge of effluents is arranged at container bottom nearby emergency effluents discharge valve if sewerage is clogged. Vibrators are mounted on one of vertical walls and body bottom with their outputs connected with control unit.
EFFECT: perfected operating performances.
SUBSTANCE: invention relates to a method of treating wood oil, particularly tall oil. The method of treating wood oil, which contains fatty acids, sterols and compounds with alcohol groups, in order to increase output of fatty acids and make easier further treatment of sterols, where said wood oil is formed during sulphate pulping of fibrous raw material, is characterised by that a low molecular weight carboxylic acid is added to the wood oil in amount of about 0.5-5.0% of the weight of the wood oil before a considerable number of alcohol groups are esterified by fatty acids initially contained in the wood oil, for esterification using said acid of at least some of the alcohol groups present in the wood oil, and for significant prevention of esterification of said alcohol groups by fatty acids initially contained in the wood oil.
EFFECT: invention increases output of fatty acids and makes easier further treatment of sterols.
SUBSTANCE: gum is treated with one or more enzymes having PLA activity at temperature of about 40-60°C and pH of about 3-7 for not more than 4 hours, which leads to formation of lysophospholipids and free fatty acids. Gum is treated with one or more enzymes having PLC activity at temperature of about 40-80°C and pH of about 8 or lower for not more than 30 minutes to form diacylglycerols and phosphates.
EFFECT: diacylglycerols and free fatty acids formed from independent reactions are combined in the presence of not less than one of said enzymes to form novel triacylglycerol molecules.
22 cl, 8 dwg, 9 tbl, 16 ex
SUBSTANCE: method of increasing output of tall oil soap from black liquor, involving adding a separation-promoting additive to black liquor, said additive being selected from a group consisting of alkyl alcohol alkoxylates of formula RO[(CH2CHCH3O)x(CH2CH2O)y]M and combinations thereof, where R is a linear or branched alkyl containing about 8 to 22 carbon atoms, x ranges from 1 to 20, y ranges from about 20 to about 80 and M is H or an alkali metal.
EFFECT: invention enables to increase output of the product when separating tall oil soap from black liquor.
12 cl, 2 tbl, 1 ex
SUBSTANCE: invention relates to a wood preservative and preparation method thereof. The preservative is crude tall oil from which neutral components have been removed, where said neutral components act as a culture medium and a feed source for saprogenic fungi and/or compounds which induce esterification reactions.
EFFECT: obtaining an effective preservative.
SUBSTANCE: invention concerns oil and fat industry. Automatic fat separator has a container and pipes for carrying the water and fat mixture and draining purified water. Connection pipe is made in form of an inlet pipe and the container is fitted with a fat-retaining inlet partition which retains a layer of fat on the surface, a fat-retaining outlet partition placed on the connection pipe carrying pure water, which is made in form of an outlet pipe through which the liquid is taken out for further purification, and an outlet pipe for the collected fat placed in front of the fat container, where the container also has a sealed top cover, one or more discs made from hydrophobic and oleophilic material, a geared motor with controlled rotational speed, a periodically switched liquid heater which heats the liquid to 55°C to provide rotation of one or more discs on which the floating heated fat sticks, and for removal and collection of fat, the device has oil removers fitted higher than the level of the liquid and the outlet pipe for the collected fat.
EFFECT: design of a device which is efficient for separating fat, simple to make, use and repair.
FIELD: technological processes; food products.
SUBSTANCE: invention is related to fat-and-oil industry. Method includes heating of soap stock, addition of electrolyte and demulsifier in it in process of mixing, separation of fat component, settling. When soap stock is heated up to 50-60°C, sodium chloride is introduced in it as electrolyte in amount of 2-6% from initial raw materials, as demulsifier - surface-active OP-7 in amount of 0.1-0.7% from initial raw materials, additionally mixture of isoamyl and isobutyl alcohols is introduced with the ratio of 2.5:1, in amount of 20-40% to mass of soap stock, and heating continues for 3-5 minutes.
EFFECT: more efficient separation of silicate soap stock fat emulsion and yield of fat component, intensification of separation process, reduction of power inputs.
1 tbl, 3 ex
FIELD: food industry.
SUBSTANCE: invention refers to food industry. The method proposed envisages injection of solid byproducts of mustard oil production into a reservoir filled with water, agitation to generate a dispersed system that is subsequently heated, maintained at the heating temperature during 15 minutes and additionally treated to provide for generation of vapour phase eventually delivered for condensation and separation. The maximum content of water the solid products are mixed with in the system is 30%; the additional treatment proceeds under pressure-tight conditions.
EFFECT: energy efficiency combined with the process acceleration.
FIELD: technological processes.
SUBSTANCE: solid wastes are loaded into reactor, and water is added for extraction at the temperature of 75-95°C, ratio of water and wastes makes 6:1 and mixing time is 30 minutes. At that mixing is carried out by means of continuous discharge of generated extract from reactor and return to it. After 30 minutes have expired, extract is discharged from reactor for mixing with the new portion of solid wastes with simultaneous addition of new portion of water for extraction to reactor that corresponds to this amount. Generated extract is divided into phases, solid phase is dried, and liquid phase is evaporated and sinigrin thioglycoside crystals are prepared.
EFFECT: intensification of process of mustard-oil production solid wastes recycling and preparation of product with good shelf life.
1 dwg, 1 tbl
SUBSTANCE: invention relates to a method of extracting alkyl-glycerine ethers having high biological activity from marine fats. The method involves alkaline hydrolysis of fat, acidification of the mixture, washing the mixture with water, first crystallisation of the mixture in an organic solvent, filtration, drying, second crystallisation of the intermediate product from the organic solvent, filtration and drying. The organic solvent used during first and second crystallisation is hexane or acetone and during the first and second crystallisation, the fat mixture is held in the organic solvent first for 12 hours at room temperature and then for 12-15 hours at 0-4°C, where during the first crystallisation, the ratio of the fat mixture to the organic solvent is equal to 1:10 kg/l, 1:50 kg/l during the second crystallisation, for hexane and 1:10 kg/l for acetone.
EFFECT: invention obtaining end products with high degree of purity and high output using an efficient and cheap method.
4 cl, 8 ex
SUBSTANCE: method involves boiling and filtration. Boiling is carried out at 100°C with simultaneous exposure to ultrasound vibrations which are directed from bottom to top at frequencies which give rise to cavitation effect which destroys all pathogenic microorganisms and creates a flotation concentration mode which carries all colloidal suspensions to the surface in form of foam which is continuously removed.
EFFECT: invention reduces expenses on purifying wax from mechanical impurities, colloidal suspensions, and enables complete disinfection of wax in a single step at low temperature while preserving the initial structure of the wax.
SUBSTANCE: method of processing pine tree bark involves extraction of the bark using a non-polar solvent with extraction of coniferous wax, subsequent extraction of pectin from the bark and treatment of the bark residue in activated carbon. After extraction of coniferous wax, the bark residue is extracted with 15% aqueous ethanol at boiling temperature for 0.5 hours. The extract is then filtered off, concentrated, saturated with sodium chloride and the obtained precipitate is separated. The filtrate is extracted with acetylacetate three times, concentrated to 1/8 of the initial volume and proanthocyanidins are settled with chloroform. The extraction agent used to extract pectin is 1% aqueous solution of hydrochloric acid.
EFFECT: method enables virtually complete utilisation of pine tree bark to obtain coniferous wax, proanthocyanidins, pectin and activated carbon.
1 dwg, 1 ex
SUBSTANCE: method involves vacuum drying at temperature of 76-120°C and excess pressure of 10-200 mmHg of a fat-wax mixture. The mixture is cooled to 4-40°C in 5-72 hours and the precipitated wax crystals are separated.
EFFECT: invention enables recycling without using chemical additives.
6 cl, 4 ex
FIELD: process engineering.
SUBSTANCE: proposed method consists in deoling sheep fleece in two steps. First, fleece is turned about and arranged on screen filter wall inner surface with wool sheared ends to be pressed by the other wall of said screen filter. Then, lateral sides of foggy belly part and fleece are bent inside, together with case walls, and locked in said position. At the second step, the case with fleece wool is bent along the working surface radius and, the case faces being connected, located concentrically inside the drum. Lower rotational speed is cut in and fleece wool is heated. Now, rotational speed is increased to remove melted wool fat with fluid working agent, produced in revolving drum, from fleece wool fibers and pumped out for further packaging and treatment.
EFFECT: higher quality of wool fat, reduced labor input.
FIELD: technological processes; chemistry.
SUBSTANCE: method of cedar bark integrated processing is described, which includes extraction of bark with nonpolar dissolvent with extraction of coniferous wax, further extraction of anthocyanidin colouring agent from bark and processing of bark remains into active coal, at that after preparation of anthocyanidin colouring agent bark remains are subjected to extraction with 0.4-1.0% aqueous solution of ammonium oxalate at the temperature of 95-100°C with extraction of pectin.
EFFECT: suggested method provides achievement of practically complete utilisation of cedar bark with preparation of coniferous wax; anthocyanidin colouring agent; pectin and active coal and makes it possible to increase pectin output and its quality.
1 dwg, 3 tbl, 6 ex
SUBSTANCE: present invention concerns chemical processing of wood, particularly fir bark, with obtaining resinous wax, tanning substances and activated carbon. A method of fir bark processing is described involving milling fir bark, extraction by non-polar solvent to obtain resinous wax, processing bark remainders with water-alcohol mix containing 1% mass units of sodium hydroxide to obtain tanning extract, and further processing solid bark residues to activated carbon.
EFFECT: almost complete utilisation of fir bark, expanded range of products made thereof at higher tanning extract yield.
2 tbl, 1 ex