Preparation of essential oil from oak moss (rubber)

Contents

Introduction

Characteristics of raw materials

Methods of isolation of essential oils

Selection of main process equipment

Process Diagram Description

Use of essential oils

Conclusion

List of used literature

Introduction

In recent years, synthetic fragrances have become important for the manufacture of fragrances for toilet soaps, synthetic detergents, plastic products, leather substitutes and many other food and chemical products. Of the fragrances currently produced by the domestic industry, 80% are synthetic.

The proportion of synthetic fragrances used in cologne compositions is about 75%, and almost 90% in toilet soaps and synthetic detergents. in food aromatic essences - about 80%.

The perfume and cosmetics industry arose in Russia in the 40s of the last century. Almost all enterprises were in the hands of foreign capitalists, there was no raw material base in the country, production was at an extremely low technical level. Essential oils, synthetic fragrances, finished compositions were imported from abroad.

Essential oil plants attracted the attention of people from ancient times. Cultural monuments of distant eras indicate that their development in different parts of the world took place simultaneously and had its own characteristics. It is known that the Egyptians 6 thousand years before the present day knew how to obtain turpentine and other fragrant substances from plants, used them in ritual rites. Long before our reckoning, the Indians mastered the simplest ways to obtain fragrant waters. In Japan, more than 2 thousand years ago, not only mint oil was received, but also menthol was isolated from it. However, this knowledge spread very slowly. The consumption of fragrant waters and plants, essential and especially incense populations in the ancient world reached its heyday and gained a truly enormous extent during the decline of the Roman Empire.

The next, medieval, stage in the knowledge and use of fragrant plants is associated with the period of development of alchemy in the VIII-X centuries. Alchemists and the search for a "life elixir" paid much attention to essential oil plants. With the advent of a special medical direction of alchemy, essential oils began to be widely used for therapeutic purposes. The first list of 56 essential oils was published in the Nuremberg Pharmacy Tax in 1454. By the middle of the 18th century. another 24 essential oils were obtained. At this time, anflerage and the mechanical method were added to the methods of processing plants by distillation and maceration, and in the second half of the 19th century - extraction with volatile solvents; many essential-mastic plants began to be cultivated in culture.

Currently, about 200 names of essential oil plants are used for the production of essential oils. The world production of essential oils from cultured and wild ether carriers ranges from 20-25 thousand tons per year, depending on climatic conditions and market conditions.

Characteristics of raw materials

Oak moss. The term "oak moss," rooted in the essential oil industry and trade, refers to the lichen Evernia prunastri Ach. the Usneaceac family, which grows not only on oak, but also on other deciduous and coniferous trees, shrubs. Oak moss is widespread in the European part of Russia.

Lichen Evernia prunastri Ach. It is a strongly branched, slightly flattened, soft to the touch of a bush - a layering. Branched, flat, ribbon-shaped blades with a strongly folded surface 2-10 cm long, wide at the base and in the middle from 1 to 4 mm extend from the base by which the layering is attached to the bark of the tree - the substrate. At the ends - less than 0.5 mm. The edges of the blades wrap downward, in places whitish rounded or elliptical powdered bundles of spore formations are noticeable on them. The color of the lichen on the upper, more convex side is grayish green, on the lower, more concave - greenish-whitish or yellowish sometimes with a pink tint. The smell is pleasant, aromatic, musknolavand with the predominance of a tepid moss note, appears after drying and storage under certain conditions.

Fragrances and lichen acids are uniformly dispersed within the cells of the laminate.

The industrial raw materials of oak moss are dried lichen layers separated from the bark of the tree, growing on the trunk and branches of oak and other hardwood, with a humidity of no more than 12%.

Since ancient times, from tree moss, like any other plant, people have tried to benefit. This was especially successful for North American Indians, who used tree moss extract as a medicine for inflammation, rotting wounds and respiratory diseases. The gallant French found their use in wood moss: back in the 1617 century, moss were collected, dried, pushed into small powder and sprinkled wigs on them. Oak moss powder not only perfectly disinfected not too tidy wigs of that time, but also gave them a pleasant aroma. Perfumers could not help but notice this, and already in the 19th century extracts and essential oil of wood moss appeared, from which perfumed water was made.

At first, wood moss was collected in Provence, where many old oaks grow in mountainous areas, and Grass perfume enterprises were engaged in processing. Over time, stocks of raw materials were depleted, and tree moss began to be imported from the countries of the former Yugoslavia, from North Africa, and today the largest part of essential oil and extract of tree moss for perfume and cosmetic needs is mined in the USA and Bulgaria.

However, the shortage of oak tree moss forced manufacturers to pay attention to a lichen very similar in aromatic properties - Pseudoevernia furfuracea, which often grows on pine and other coniferous trees, and resinous notes are clearly heard in its smell.

In our country, oak moss is extracted with ethyl alcohol. The resulting extract is called a resnnnoid. The yield ranges from 9.5 to 13.0%. The resinoid composition includes various lichen acids and their esters with ethyl alcohol, which are odorless, but have fixing and antimicrobial properties, geraniol, ztronellol, vanillin, camphor, znneol, borneol, etc.

Lichens are perennial lower plants consisting of two organisms: fungus and algae. Nutrients are formed due to photosynthesis by algae and are obtained by the fungus from the substrate. Water is absorbed by them mainly in a drip-like state from fog, dew, rain, water vapors and only partially comes from the substrate. These biological features determine the effect of various factors on the yield and quality (composition) of the rubinoid.

The substrate has the most significant effect. Thus, the yield of rubber from lichen from oak bark is 9.8%. Beresta - 16.8%, wild apple trees - 26.7%. The yield of rubber from lichen growing in shade is less than in the sun.

The best in odor and content of ballast substances rubber can be obtained from lichen from birch bark; the lowest perfume rating is characterized by lichen rubber from coniferous trees.

The quality of the rubinoid depends on the age of the substrate. It increases when lichens grow on old trees and branches older than 15 years.

The composition of lichens changes within a year. Due to this, in the summer, the perfume estimate of rubinoid from lichens from any trees, with the exception of birch bark, is reduced.

The yield of the rubber is increased during long-term storage.

The supplied oak moss raw materials must correspond to the external characteristics described above: have a weak, pleasant smell; slightly acidic taste, moisture content is not more than 12%; contain mineral impurities not more than 0.5%; organic impurity, except lichens, not more than 1.0%; foreign lichens not more than 3.0%; impurities of this lichen - bushes, the bases of which are not released from the remains of the bark of the tree - not more than 5% and crushed parts passing through a sieve with a diameter of holes of 3 mm, not more than 5%.

The absolute of oak moss has been most widely used in the creation of perfumes. The finest, refined, but at the same time very strong and persistent aroma of oak moss extract perfectly captures other odors, and therefore is used as basic notes when creating luxury luxury perfume compositions, especially spike, fusher, oriental and aldehyde directions (for example, Chanel No. 5 from Chanel, Miss Dior from Dior, Opine, Lalimar from Langer from Luar.

Physical characteristic:

1. Absolute is a dark green or brown very viscous liquid with a strong smell of moss and earth.

2. Oil from absolute - pale yellow or olive liquid with the aroma of bark and earth.

3. Concretes, resins and rubinoids are dark hard or viscous masses with a persistent, heavy earth aroma.

The rubber extract was to have the following specifications:

- density 0.9800.998,

- acid number 2030,

- ether number 1520,

- content of precipitate, insoluble in alcohol, not more than 6%,

- content of ethyl alcohol is not more than 15%.

If necessary, the rubber was clarified by sorption. To obtain a product like an absolute European oil, the rubber is dissolved in ten times the amount of alcohol, the precipitate is separated and the alcohol is distilled off.

Absolute oils of Yugoslav origin (according to J. Terajima) on average contain 21% fiscianin and 0.2 to 7% evernic acid ester.

The biomedical properties of the European oak moss extract (specifically) were studied by RIFM in 1973. The acute toxicity was: oral LD50 2.9 g/kg (rats), derm. LD50 > 5 g/kg (rabbits). In the form of a 10% solution in petroleum, the concretus does not cause irritation of the human skin and a sensitization reaction in 48 hours. There is no phototoxic effect. IFRA limits the 3% use of oak moss extracts in perfume compositions .

Methods of isolation of essential oils

Essential oil raw materials are processed by physicochemical methods and mechanical methods. The first include distillation of essential oils with steam, extraction with volatile solvents, extraction with non-volatile solvents (maceration), sorption with various sorbents (anflerage and dynamic sorption); mechanical method is carried out by pressing or scraping.

The choice of the processing method depends on the property of the raw material, the type of essential oil stores, the composition of the essential oil and the properties of its components, the nature of the connection of the essential oil with the raw material. If the essential oil is in the bound state, the fermentation of the feedstock either precedes or is combined with the main processing process.

The chosen method should ensure the highest yield and the best product quality.

Distillation of essential oils with steam

Steam distillation is the most common method for producing essential oils. Based on the volatility of essential oils with water vapors, it is carried out at atmospheric pressure at a temperature of about 100 ° C. Such a low recovery temperature of oils, whose components have a boiling point in the range of 150-250 ° C, is one of the main advantages of the method.

The essence of the method lies in the fact that when treating essential oil raw material with steam, the components of essential oils are transferred to the vapor phase and in the mixture with water vapors are sent for condensation, and then for separation from water.

The ethereal oil processing scheme below is simple.

The raw material, whole or crushed, is charged into a distillation apparatus into which steam is supplied. Steam in contact with the raw material extracts essential oil. The resulting mixture of essential oil vapors and water from the distillation apparatus is withdrawn to a refrigerator in which vapors condense and the distillate is cooled to a predetermined temperature. Distillate is supplied to the receiver oil separator (florentine), where it is settled and divided into primary essential crude oil and distillation water.

In the distillation water, a certain amount of ether oil remains in the dissolved and suspended states, which is recovered, as a rule, by re-distillation (cohabitation). At the same time 4-30% of secondary distillate is distilled off and secondary essential crude oil is obtained.

Raw oil contains water in dissolved and suspended states. It is dewatered by settling, vacuum drying or combination thereof. Fine raw material particles and other mechanical impurities in oil are separated by filtration.

Essential oils, such as anise and mint, are necessarily subjected to re-distillation with steam to improve the smell, taste and color. In the practice of essential oil production, this process is known as steam rectification. In this process, essential oil is enriched with the main component and ennobled: light-volatile substances with an unpleasant smell, bitter taste and difficult-to-fly, dark-colored substances are released from it. The oil after re-distillation is called the essential rectificate oil.

In our country, much attention is paid to the development of this ancient method. 90% of raw materials are processed on continuous devices, the designs of which are constantly improved. The method is supplemented by waste processing for the full use of raw materials.

Further improvement of the method is aimed at improving the quality and output of essential oils, at developing technological lines for the integrated use of raw materials.

The advantages of the method: simplicity, relatively low process temperature, fire safety, high labor productivity, harmlessness.

Disadvantages include the deterioration of essential oils due to chemical changes of components, especially terpene alcohols and esters thereof. and loss of valuable fragrances not volatile with steam.

Extraction with volatile solvents

Extraction with volatile solvents is increasingly used in the ether-oil production.

The method is based on the solubility of plant fragrances in organic solvents and liquid carbon dioxide. In addition to essential oils components, hardly volatile resinous substances with fixing properties, interesting odors, and waxy substances are extracted from the raw materials. The extractconcret is obtained, the yield of which is always higher than essential oil, and the smell more fully transfers the aroma of plants due to the extraction of the entire complex of fragrances and the absence of chemical changes in the components.

Increased yield, high quality of extract oils "high economic production indicators make up the main advantages of the method.

Essence of method lies in treatment of ether-oil raw material with solvent by immersion in it or by irrigation. Extractable substances are transferred to solvent. solvent is distilled from the resulting solution (miscella) to obtain an extractconcret.

The scheme of treatment of essential oil feedstock is presented below.

The extraction process is most often carried out by petroleum ether or extraction gasoline A at ambient temperature, in some cases at 40-50 ° C. The raw material is charged into an apparatus (extractor) into which the solvent is fed. The resulting solution of a particular (miscella) concentration of 0.1-0.3% is subjected to two-stage distillation: at the first stage, under atmospheric pressure, the remaining solvent is strengthened to a concentration of 8-30%, at the second stage, under vacuum.

Solvent retained by extraction wastes is regained by steam distillation. Specifically, in general, perfumes are not used because they contain waxy substances insoluble in ethyl alcohol. Therefore, an alcohol-soluble part known as an absolute oil is isolated from them by an extraction method, which is based on the different solubility in ethyl alcohol of the components of the absolute oil and waxes at a reduced temperature.

The absolute oil is isolated as follows: the extracts are dissolved in ethyl alcohol at ambient temperature or under heating. The resulting solution was cooled and held for wax crystallization. The mass is then filtered under vacuum. The filtrate, which is an alcohol solution of absolute oil, is sent for vacuum distillation. After distilling off the ethyl alcohol, an absolute oil was obtained. Waxes are additionally treated with ethyl alcohol in order to fully extract absolute oil, then they are subjected to special treatment and cosmetic waxes used in decorative cosmetics are obtained.

Some of the feedstocks in the fixative group, which are almost volatile-free, are extracted directly with ethyl alcohol. These include oak moss and incense.

In our country, extraction of essential oil raw materials is carried out mainly in a continuous way. The method itself, individual processes of the technological scheme and the corresponding technological equipment are constantly being improved.

It has been proved that 10-30% more essential oil is extracted from the raw material than in steam distillation. In this regard, research is currently underway and the issue of obtaining essential oils by extracting the raw materials and then separating them from a particular one is being considered.

The new technology for the production of essential oils is characterized by high economic indicators.

The development of the method is intended to be carried out in a wide range, not limited to the extraction of only fragrances. Essential oil raw materials can serve as a source of production of a number of products necessary for the national economy. First of all, these are biologically active substances.

The complex use of raw materials is an urgent task of the essential oil industry, and the development of the extraction method will help to successfully solve it.

Extraction with non-volatile solvents

The method of maceration, or extraction with non-volatile solvents, historically preceded the method of extraction with volatile solvents. This is one of the oldest methods of extracting fragrances from plants. They process only flower raw materials.

The method is based on the solubility of fragrances in non-volatile solvents, as which high-quality animal fats (beef, pork or mixtures thereof, called corpus), vegetable fatty oils (olive, almond, bone from apricot or peach bones), difficult-to-volatile organic compounds, for example benzylbenzoate, were used.

Essence of maceration method consists in extraction of fragrance substances from raw material by non-volatile solvents by infusion and their separation from mixture by extraction with ethyl alcohol.

The flow chart consists of the following stages: preparation of solvent, infusion, separation of lipstick or incense (antique) oil, extraction of flower extract, production of flower oil, regeneration of solvent from processed raw materials.

Flowers are immersed in the solvent heated to a given temperature and held for a certain time (up to 48 hours), the duration of which depends on the type of raw material, solvent and temperature. Upon completion of infusion, solvent is removed from the mass, which is immediately used for the next infusion of fresh raw materials. The change of flowers is carried out up to 25 times. At the end of the process, the fragrant-saturated solvent was dried with anhydrous sulphate omotarium and filtered. The resulting product, when used in animal fats, is called lipstick, when using vegetable fatty oils or hardly volatile substances, is called incense oil. They are used directly in cosmetics, and incense oils prepared on hardly volatile organic compounds soluble in ethyl alcohol are used in perfume compositions.

In most cases lipsticks and incense oils on. vegetable fats are treated with ethyl alcohol, alcohol extract (flower extract) is used directly in perfume or flower oil is obtained from it by distillation of ethyl alcohol under vacuum. Flower extracts are produced under numbers reflecting the amount of raw materials in kilograms consumed for the preparation of 10 liters of extract.

Flower oil from lipstick differs from absolute oil from the same raw material by the presence of ballast substances extracted by ethyl alcohol from a non-volatile solvent. Due to this, it has a solid consistency.

Due to the high consumption of high-quality fats, high labor intensity, insufficient extraction of fragrant substances, maceration gave way to extraction with volatile solvents.

Sorption method of extracting essential oils

The sorption method differs in that it allows to obtain more essential oil from the raw material than is contained in it when entering for processing, due to the combination of physical and chemical processes of extraction with ongoing biochemical processes of oil formation.

The method is used for those types of raw materials in which the oil formation processes do not stop after harvesting. These include the flowers of large-colored jasmine, tuberose, lily, etc. Of the first two, the oil yield by this method can exceed the content at the time of cleaning by 11-12 times.

The method is based on the ability of animal fats, vegetable fatty oils, non-volatile organic substances and some solid sorbents to absorb fragrances from the air.

The essence of the method lies in the fact that fragrant substances are released from flowers placed in a closed space into the air, which are sorbed in a gaseous state by liquid or solid sorbents, and then extracted from them by extraction with a volatile solvent.

The method is carried out in two ways depending on the nature of the sorbent. According to the first, long known as "anflerage," a body of fats is most often used as a sorbent, as well as vegetable fatty oils or hardly volatile organic compounds (the same as in maceration); first, lipstick or incense oil is obtained, respectively. By treating the semi-products in the same way as in maceration, flower extract and absolute lipstick oil are obtained. It is valued above lipstick flower oil by the maceration method.

In the process of anflerage, special wooden frames (chassis) with dimensions of 50x50 cm and 90x60 cm are used, 5-8 cm thick with thick-walled windows inserted into the middle. A thin layer (3-5 mm) of the body is applied to both surfaces of the glass. Prepared chassis is installed in horizontal position and raw material is poured on glass with layer not exceeding height of side. Chassis with raw materials are superimposed on each other for 30-l40 pcs in batteries. Raw material in batteries is located in closed chambers between two layers of the body. After 12-72 hours (depending on the type of raw materials), the flowers are shaken off, adhered to the body are removed with tweezers. Body is overblown and leveled. Chassis is turned over, loaded again with a portion of fresh raw materials and installed in batteries. The amount of feed shifts depends on the absorption capacity of the housing and reaches 30.

The saturated body (lipstick) is removed from the glass, melted and filtered into containers. Lipstick is assigned number, numerical value of which, divided by 10, reflects consumption of raw materials in kilograms per 1 kg of hull.

The use of the housing makes the process extremely labour intensive.

In case of anflage with liquid sorbents, chassis glass is replaced with metal nets, on which pieces of bulk fabric impregnated with sorbent are laid. Antique oil is extracted from fabric by pressing followed by extraction with ethyl alcohol to produce flower oil.

Liquid sorbents simplify the process, but reduce the yield of the target product.

According to the second method of the adsorption method, developed by Soviet specialists and called dynamic sorption, the sorbent is birch active coal; the ether oil extracted by extraction with diethyl ether from coal is called adsorption oil.

Anflerage and dynamic sorption are carried out at ambient temperature. After sorption, part of the volatile and the entire complex of valuable non-volatile substances remain in the flowers. Therefore, they are extracted with petroleum ether and, according to the first method, a concret and absolute oil from the chassis are obtained, according to the second method, a concret and absolute after dynamic sorption.

Mechanical method of extracting essential oils

The mechanical method is used to process the fruits of citrus crops (bergamot, lemon, mandarin, orange, pampelmus), in which essential oil is located in large readily available essential oil collars located in the surface tissues of the peel.

The method is carried out in two ways: scraping or rubbing whole fruits, in which the surface of the peel is destroyed; by pressing whole fruit or one peel separated from the pulp.

On modern lines for the processing of citrus fruits, juice, essential oil and pulp or pulp processing products are immediately obtained: pectin, citric acid, bioflafons, fatty oil, livestock feed, etc.

The essential oil obtained by the mechanical method is not exposed to heat and therefore has a natural aroma. But citrus oils contain a lot of hydrocarbons (up to 90%), limiting their solubility in ethyl alcohol, which is very important in perfume production. Therefore, citrus essential oils are deterpenized (enriched with oxygen-containing components) using vacuum distillation or liquid extraction with paired solvents.

The yield of essential oil from whole fruits of orange is 0.30-0.35%, lemon - up to 0.60%, tangerine - 0.20-0.35%, bergamot - 0.38%.

Essential oils of citrus fruits are widely used in the perfume and cosmetic industry and in various branches of the food industry.

The mechanical method is used in countries with developed production of citrus fruits, such as the USA, Italy, Portugal, Spain, etc.

Selection of main process equipment

Raw material grinding

Essential oil raw materials in the form of inflorescences and branches must be ground before processing on continuous devices. The optimum particle size depends on the kind of raw material. Initially, agricultural machines were used for this purpose (power cuts RSS6 and Volgar 5). Each of them serves one set. These machines do not provide the necessary particle size of the raw materials, often fail, causing stops of distillers and additional oil losses, and require heavy physical labor. Currently, the RSSb and Volgary5 silos are everywhere replaced by special shredders (ITR, Era, DKUM, etc.). If it is from essential oil, it is therefore accompanied by losses of essential oil. The greater the loss, the more the air blowing the surface of the particles.

The DKUM grinder, which is characterized by high productivity (from 8 to 10.8 t/h), is used in the scheme we have chosen.

Grishin-Sheshalevich extractor:

The process flow diagram of raw material processing by extraction method includes processes of extraction, distillation of miscella and extraction of absolute oil from a particular one.

Until recently, the ether oil feed was extracted only by immersion. This method is characterized by a high ratio of solvent to raw materials and a low rate of extraction of extractable substances.

In recent years, the extraction of essential oil raw materials by the irrigation method has been mastered, which has shown excellent results in the processing of raw materials. The process is carried out in a vertical apparatus in countercurrent flows of the liquid and vapor phases of the solvent. The extractable raw material is moved from the bottom up, irrigated from above with a heated solvent, countercurrent to which vapors of the same solvent move. Introduction of solvent vapour flow into extraction zone ensures uniform distribution of liquid phase along section of apparatus and turbulisation of flows at phase interface.

The process is carried out in a closed cycle at a temperature of 45 - 50 ° C, with the ratio of solvent to raw materials (0.5 -2.0): 1 l/kg.

The turbulent mode of movement of the liquid phase and the elevated temperature intensify diffusion processes, prevent sorption phenomena. As a result, the speed and degree of extraction of extracted substances increase, the duration of the process "increases by 5-7 times the specific productivity of the extractor. Compared to extraction by immersion in Grishin-Sheshalevich devices, the yield specifically increases from 0.82 to 1.48%, from waste - by 70%. All this indicates the advantages of irrigation extraction.

Oak moss with a capacity of 200 250 kg/h are processed on apparatus of Grey Sheshalevich.

Separation of absolute oil from a particular

The isolation of absolute oil from a particular one is based on the different solubility of absolute and wax components in high concentration ethyl alcohol at a reduced temperature or in diluted alcohol at ambient temperature. It is produced in several ways.

The first way. The concrete in the reaction apparatus is dissolved in 96% ethyl alcohol in a ratio of 1 kg: 8 l for 10-12 hours with stirring at a temperature of 42-45 ° C. The resulting gel-like mass is pumped into a crystallizer with a stirrer in the jacket of which brine circulates at a temperature of -14 ° C, Wax crystallization (freezing) lasts 6-7 hours with stirring with 10-15 minute pauses every 30 minutes. Upon completion of crystallization, the mass is drained by gravity onto a nutfilter cooled with brine, where alcohol miscella of absolute oil is filtered under pressure of 21.3-26.6 kPa for 9 hours at crystallization temperature of -14-17 ° C.

During filtration, the state of the mass on the filter is monitored, the cracks that appear are covered with a blade to avoid vacuum loss to the alcohol mnecella with absolus waxes. Waxes isolated during filtration are dissolved in the ratio of 1 kg: 4L in 96.5% ethyl alcohol with addition of alcohol used to it. Waxes are dissolved at least 3 times. If absolute content exceeds 0.5%, dissolved waxes are continued. From the obtained miscella (filtrate) in a vacuum apparatus with a refrigerator and a receiver, ethyl alcohol is distilled off at a pressure of 5-13.3 kPa and at a liquid temperature of 42 to 44 ° C at the beginning of the process to 58-59 ° C - at the end. As the alcohol is distilled off, miscellas are loaded into the apparatus after dissolving the second and third waxes. This achieves simultaneous blending of absolute, since its composition changes in the process of alcohol extraction due to the different rate of extraction of individual components from the mixture with waxes. From treated waxes ethyl alcohol is distilled off in the mode of alcohol miscella absolute distillation. The amount of alcohol exceeds the dry weight of waxes. The oil and the concentrate has a reduced concentration, contains components that are part of petroleum ether or gasoline. Alcohol concentration is reduced due to loss of anhydrous alcohol during filtration and vacuum distillation.

Second way. This method is borrowed from foreign technology. French experts believe that the dissolution of a particular at an elevated temperature adversely affects the quality of the absolute. and it is proposed to carry out this process at ambient temperature and vigorous mixing. This requires at least 8 hours. The insoluble part of the waxes is in the form of thin light petals and is very easily separated by filtration before cooling the alcohol solution. Filtrate is directed for cooling-crystallisation of the remaining wax part. Further operations do not differ from those described above.

In addition to eliminating the undesirable long-term thermal effect on the absolute, this technique improves the structure of waxes crystallizing when the alcohol solution is cooled, and significantly reduces the filtration time. Despite the two filtering, the total time is less than 2 times.

A prerequisite for this dissolution process is specifically a highly effective mixing.

The third way. This method is based on the use of diluted ethyl alcohol with a concentration of 60%. The process is applicable to oils in which there are few volatile compounds soluble in dilute alcohol. Method is used for isolation of absolute from particular and extract from wastes of nutmeg sage. Absolute dissolves in 60% ethyl alcohol, and waxes float and are separated by decantation. Alcohol miscella absolute is strengthened by distillation of alcohol, while it delaminates: the upper layer is absolute, the lower layer is 30% ethyl alcohol. After drain of lower alcohol layer vacuum-drying of absolute is performed.

There is no vacuum filtration in the scheme, it is extremely simple. However, the oil yield in this process is significantly lower than in the first.

A new way. This method, which is fundamentally different from all of those discussed, is based on isolating the absolute from concentrated miscellas specifically in petroleum ether or gasoline by liquid extraction with aqueous ethyl alcohol. The optimal concentration of miscella is specific 7-10%, ethyl alcohol - 87-90%, the ratio of miscella to alcohol is 1:1. The method has the following advantages: eliminates the stage of vacuum treatment of concentrated miscellas specifically; increases absolute yield by reducing wax loss; improves the quality of the absolute by eliminating losses with a distillable solvent during vacuum treatment of the miscella of a particular one; reduces the consumption of ethyl alcohol by 28-47%; the process is carried out in continuous mode, which reduces the time required to obtain the absolute by 6-10 times; absolute production is combined in time with the processing of raw materials, that is, storage is eliminated specifically.

Process Diagram Description

In industry, oak moss is extracted in continuous and periodic devices. According to the continuous extraction scheme, the raw material is crushed on a DKUM 21 crusher into particles of 2-3 mm size, air transport is supplied to cyclone 23 and 10-15 kg are fed from it in portions through 20-30 minutes to the first extractor 1. The raw material passes sequentially two Grishin-Sheshalevich extractors for 5 h 40 min in countercurrent to ethyl alcohol. 2-3 l of ethyl alcohol is fed per 1 kg of raw material. Process temperature 74-76 ° C. It is provided by heating the alcohol entering the devices and the devices themselves with the help of steam jackets available in the lower part. The alcohol is heated in the heat exchanger 26 and fed to the extraction column of the second apparatus 2. The resulting alcohol vapors condense in the reverse coolers 24 and 27. The capacity of the plant is 700-1000 kg of raw materials per day.

The post-extraction waste containing 30% ethyl alcohol and 0.04-0.10% rubber from the second extractor 2 is fed to the feed screw of the evaporator 5. The evaporator arrangement provides good mixing of waste and contact with steam which will be supplied to the lower part of the evaporator. Vapors of alcohol and water enter the cooler 4, from which the distilled alcohol with a concentration of 70% is drained to the dilute alcohol collector 6 and then sent to rectification by the pump 7 for strengthening up to 96%. Wastes from evaporator by conveyor 5 are fed into hopper and removed.

Miscella from the feed column of the first extractor is cooled in the heat exchanger 22 to 30-40 ° C and sent by gravity in turn to the settling tanks 19, 18 and 17 to settle and separate the insoluble precipitate. Settling lasts up to three days. The precipitate is periodically lowered into the collector 20. The settled mnecella is cleaned on the filter 16 and sent to the evaporator of the first stage 15, in which it is strengthened to 14-18% under atmospheric pressure and temperature 78-80 ° C. Overheating the miscella at this stage leads to caramelization of carbohydrates, an increase in the color of the finished rubinoid. The alcohol distilled at the first stage with a concentration of 92-96% from the refrigerator 14 enters the strong alcohol collector in and without strengthening is used for extraction, it is supplied by the pump 9 to the pressure tank 25. The evaporated miscella is sucked into a vacuum apparatus 13, in which, during steam-water heating, the alcohol and water are finally distilled under a pressure of 9.3-13.3 kPa to a temperature of not more than 60 ° C. The distilled alcohol under vacuum enters the refrigerator 12 and is transported from the vacuum receiver 11 to the weak alcohol collector 6.

The resinoid discharged from the vacuum apparatus has a very viscous consistency that is inconvenient for packing. Therefore, it is mixed with fresh 96% alcohol in an apparatus with a stirrer and jacket 10 while heating to 30-33 C and stirring.

Periodic extraction. It is carried out by three times infusion, the first two - 3 hours each and the third - 2 hours. The total extraction duration is 10 hours, including the time of filling the apparatus with solvent and draining miscella. The first infusion is carried out with a miscella of the second infusion from previous feedstocks; the second - washing mscell of the third infusion; fresh solvent is used for the third infusion (washing). Alcohol concentration 90-96%. The process temperature is 60-65 ° C.

Periodic extraction is carried out in overturns of PK1500 type with steam jacket, sharp steam bubbler and intermediate removable metal grids. 150-170 kg of non-ground moss is loaded into the apparatus and solvent is supplied from bottom to top by centrifugal pump. Upon completion of infusion, the first miscella is drained and settling tanks through a horizontal heat exchanger for cooling to 18-20 ° C. The settling and treatment of the miscella is carried out in the same way as with continuous extraction. The second and washing miscellles are drained into separate collectors and used for extraction of new portions of raw material. From the waste, ethyl alcohol is distilled away first with deaf steam, and at the end with deaf and sharp steam. The concentration of distilled alcohol is 30-70%. Rubber losses in wastes 0.4%.

Brightening of the rubber. The intense color of the rubber is adversely affected by the color of perfume liquids. Clarification is carried out by sorption of pigments from 10% solution of reznoid in ethyl alcohol. The sorbent used is a copolymer of Nvinylpyrrolidone with triethylene glycol dimethacrglate (P-3). 20 g of P-3 are required per 1 liter of rubber solution. Loss of rubinoid solution during clarification 6-12%.

According to Bulgarian technology, discoloration is carried out at a temperature of - 15 ° C with the active ground "Kalosha" from a 14-15% solution of rubinoid in ethyl alcohol after cooling it to - 15 ° C and filtration.

Use of essential oils

Packaging, labelling and storage of essential oils

Dry pure essential oil is packed in containers of glass, white tin and steel, galvanized iron. When filling the tar, leave free space to avoid tightness disturbances when changing temperature. The jars are tightly sealed, the opening in the upper bottom of the tin can is covered with a larger diameter circle and is covered around the circumference. Closed jars are tested for tightness by turning them over to holding in various positions. Labels with the name of the Ministry, the manufacturer are pasted on checked rolls and cans. name of essential oil, analysis numbers, gross and net masses Tin jars are packed in wooden boxes with shavings gasket. The box is wrapped with wire. Boxes and barrels with essential oil are marked in accordance with GOST.

Essential oils packed in packagings shall be stored in replaced storage rooms at a temperature of 5 to 25 ° C and a relative humidity of not more than 70%.

Pure essential oil can be stored for two years (counting from the end of the distillation process or the date of bottling, and with clear observance of the storage regime, this period can be increased to three to five years. The average storage temperature of oils is from 5 to 25 ° C.

Water and is not allowed to enter the bottle with oil. impurities - this will quickly ruin it. Water in essential oil may appear in the form of condensate, when taken out of the refrigerator, so experienced aromatherapists do not advise storing natural aromamasles in the refrigerator.

Freshly prepared mixtures with essential oils are desirable to be used immediately, with long-term storage, the effect of their use is reduced. The resulting mixture remains suitable for about three months, provided that other components are available during this period. If you use base oil that is not prone to rancidity, this period can be increased.

If the smell of the mixture has changed, then it is no longer suitable for use. Careless treatment of esters can cause severe poisoning, burn of the skin and mucous membranes, as well as severe allergies.

Properties of wood moss used in cosmetics:

Aromatic.

The absolute of oak moss has been most widely used in the creation of perfumes. The finest, refined, but at the same time very strong and persistent aroma of oak moss extract perfectly captures other odors, and therefore is used as basic notes when creating luxury luxury perfume compositions, especially spike, fusher, oriental and aldehyde directions (for example, Chanel No. 5 from Chanel, Miss Dior from Dior, Opine, Lalimar from Langer from Luar.

Anti-inflammatory.

Wood moss extract contains elements resembling phytoncides, which are able to fight fungal infections, eliminate inflammation on the skin.

Healing.

Essential oil of wood moss accelerates the healing of wounds, ulcers, scratches, prevents their suppression.

Strengthening.

Wood moss extract contains tannins, thanks to which it tones skin cells, strengthens hair bulbs, keratin hair scales.

In folk medicine, essential oil of wood moss is used to arouse appetite, treat cough and respiratory infections, skin diseases, and even as a mild laxative.

Aromatherapy with essential oil of wood moss relieves stress and strengthens the nervous system.

The use of cosmetics with wood moss extracts is undesirable:

in case of allergy to essential oil of wood moss, in particular to elements included in its composition: tuyons, terpenes, alcohols

in the first 4 months of pregnancy

in the presence of epilepsy

Long-term storage of perfumery and cosmetics containing essential oil of wood moss can lead to the formation of oxyperoxides in its composition that can cause allergies. However, in general, the composition of the essential oil of wood moss is quite complex (it contains more than 80 elements), therefore, from the point of view of chemists, it can be allergic only in individual perception. However, the International Perfume Association (IFRA) has recognized woody moss as a strong allergen and recommends that perfume manufacturers abandon this ingredient.

Conclusion

The absolute of oak moss has been most widely used in the creation of perfumes, medicines with healing, anti-inflammatory, strengthening effects. The finest, refined, but at the same time very strong and persistent aroma of oak moss extract perfectly captures other smells, and therefore is used as basic notes when creating luxury luxury perfume compositions.

At present, it is difficult to imagine perfume products without the use of oak moss rubber, the production of which is carried out according to the scheme of continuous extraction in the extractor of Grey Sheshalevich, operating on the principle of irrigation. In this course project, the above hardware and technology scheme and equipment included in it were considered. The characteristics of the raw materials are also given, storage of the finished product and its use are studied.

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