ES2362850A1 - Procedure for enrichment of essential oils. (Machine-translation by Google Translate, not legally binding) - Google Patents

Abstract

Procedure for enriching essential oils. The present invention relates to an enrichment process of essential oils, more in particular it refers to a method able to increase the concentration of the hydrophilic components of an essential oil that takes advantage of an industrial refrigeration cycle by compression, improving the properties of said oil, said method comprising the steps of: a) passing said essential oil through a hydrophilic stationary phase; b) passing a gas through said stationary phase; c) eluting the absorbed components by passing a refrigerant in liquid state through said hydrophilic stationary phase; and d) evaporating said refrigerant. (Machine-translation by Google Translate, not legally binding)

Description

Oil enrichment procedure essential.

The present invention relates to a Essential oil enrichment procedure, more in particular refers to a procedure suitable for increasing the concentration of the hydrophilic components of an essential oil, improving the aromatic properties of said oil.

Essential oils are complex mixtures of natural molecules that are usually obtained from plants. These essential oils are secondary metabolites that can usually be obtained by extraction with organic solvents and subsequent concentration or treatments physical with steam, followed by a separation of the insoluble phase in Water. In the case of citrus fruits, these essential oils they are in glands of the skin of the fruit and are extracted by pressure or scraping of the skin with the help of water dragging and a subsequent separation of water through a centrifugation process to get the essential oil. Usually at temperature ambient are liquid, slightly volatile, soluble in organic solvents and have a density lower than that of Water.

In addition to their therapeutic properties, the Essential oils have a great industrial interest in the industry Pharmaceutical, food and perfumery. In the industry of Food is used to season prepared meats, sausages, soups, ice cream, cheese, etc. They are also used in the preparation of alcoholic and non-alcoholic beverages, especially refreshments. With respect to this utility we can cite the essences extracted from orange, lemon, mints and fennel, among others. These essences are also used in the production of candies, Chocolates and other goodies.

In the pharmaceutical industry they are used in creams Dental, analgesic and inhalants to decongest the pathways respiratory, etc. They are used in the manufacture of Unpleasant taste neutralizers of many medications. Too They are used in aromatherapy for their properties. In the industry of Cosmetics are used essential oils in the production of soaps, colognes, perfumes and makeup. Currently it has developed the use of essences to hide the unpleasant smell of some industrial products such as rubber, plastics and the paintings. They are also used in the paint industry, in textiles, stationery, toys, among many other uses.

The chemical composition of essential oils differs not only in quantity but also in quality and type of stereochemistry of the molecules of the extracted substances. He Extraction product may vary according to genotype, weather, the composition of the earth, the plant organ used to extraction, age and the vegetative cycle in which it is found plant. It also depends on the extraction procedure used.

Among the examples of chemical compounds present in essential oils are alcohols terpenics such as linalool, geraniol, tuyanol, borneol, menthol, citronellol, alpha-terpineol, finish-4-ol, nerol, etc. Phenols such as: thymol, carvacrol, eugenol, guaiac, among others; sesquiterpenic alcohols such as nerolidol, farnesol, santalol, cedrol, patchoulol, carveol, bisabolol, sclareol, among others; aromatic aldehydes such as cinnamaldehyde, cuminal, benzaldehyde, among others; aliphatic aldehydes such as octanal, nonanal, decanal, undecanal, dodecanal, among others; aldehydes terpenics such as neral, geranial, citronelal, anisal, mirtenal, among others; terpenic ketones such as verbetone, piperitone, mantona, borneona, fenchona, carvona, pulegona, among others; esters such as citronellyl formate, geranyl formate, acetate beryl, terpenyl acetate, mentyl acetate, linalyl, bornyl acetate, eugenyl acetate, methoxyanthranilate methyl, among others; terpenes such as alpha and beta pinene, Myrcene, delta-3-carene, para-cimeno, limonene, ocimeno, alpha and beta terpineno, terpinoleno, sabineno, canfeno, felandreno, among others; sesquiterpenes such as humulene, germacrene-D, chamazulene, farneseno, zingibereno, elemeno, himachaleno, cubebeno, choapeno, pachuleno, cariofileno, gaiaeno, among others and also lactones, coumarins, phthalides, nitrogen compounds and compounds sulfur

One of the main problems of essential oil enrichment procedures of the prior art is that they possess a high degree of complexity in terms of equipment and operation. In addition, they use solvents organic harmful to health and the environment, which have to be eliminated in complicated subsequent processes and always it is possible that they contaminate both the human being and the environment.

To solve the problems of the technique above, related to enrichment procedures of essential oils, the present invention discloses a new procedure in which a refrigeration cycle is used by compression, which comprises the stages of:

to)

do passing said essential oil through a stationary phase hydrophilic;

b)

do passing a gas through said stationary phase;

C)

elute the absorbed components by passing a refrigerant in form liquid through said hydrophilic stationary phase; Y

d)

evaporate said refrigerant.

With the process of the present invention, leverages the knowledge of the industrial refrigeration cycle to The enrichment of essential oils. In addition, when using a refrigerant harmless to the environment and to the human being is achieved avoid contamination caused by solvents usually used in these procedures.

It is known in the art that a cycle of compression cooling comprises the evaporation stages by expansion of a liquid refrigerant gas, which at evaporate absorbs latent heat of vaporization. Then, said refrigerant is liquefied by compression increasing the pressure of the steam for condensation. This pressure increase to achieve the change of state of the refrigerant produces an increase in its temperature, so it is necessary to cool it. In this way, the liquid refrigerant, can evaporate again by expansion and repeat the compression refrigeration cycle, usually in a closed circuit.

A refrigerant is a liquid or easily liquefiable chemical compound that can be used to serve as a heat transfer medium between a cold bulb and a hot bulb in a compression refrigeration cycle, remaining chemically stable within the cycle. Ideally, a suitable refrigerant should have the following characteristics with respect to working conditions: low boiling point, high latent heat of vaporization, low condensing pressure, freezing temperature of the liquid below the lowest working temperature, the Critical temperature and pressure must be higher than working temperatures and pressures, low specific volume, high thermal conductivity, low viscosity, chemical inactivity and stability, chemically inert (non-flammable, non-toxic, non-explosive) both pure and mixed. with air in a certain proportion and that should not contaminate the air in case of
leakage.

Another characteristic that the refrigerant to be used in the process of the present invention is that it must be able to break the hydrogen bridge bonds formed between the surface of the hydrophilic stationary phase and The components of essential oils to enrich.

Among the examples of suitable refrigerants for use in the process of the present invention find refrigerants classified as high security, whose composition does not affect the ozone layer and are allowed by legislation, such as hydrochlorofluorohalides (HCFC) and hydrofluorohalides (HFC), preferably the 1,1,1,2-tetrafluoroethane (TFE) when the product is Obtain is intended for food. Other suitable refrigerants they are R-123 (2,2-dichloro-1,1,1-trifluoroethane), R-124 (2-Chlorine, 1,1,1,2-tetrafluoroethane), R-227 or R-113, or a mixture of themselves, which can be used in non-food products. Preferably the refrigerant used in the process of The present invention is 1,1,1,2 TFE, which is included in the food regulation as an extraction solvent and that It is even accepted for some pharmaceutical uses, such as propellant in bronchodilator dispensers.

In the process of the present invention, makes the essential oil to enrich through a phase hydrophilic stationary. Said stationary phase preferably It is comprised of silica gel or alumina. In addition, said phase stationary will be contained within a suitable support for withstand high operating pressures, preferably up to 100 bar, more preferably up to 25 bar. In addition, preferably in the bottom of said support will be placed a filter in order of retaining solids particles. Preferably, step a) of The process of the present invention is carried out in a regimen of laminar flow without agitation.

Silica gel is one of the phases stationary most commonly used for product separation Natural in the laboratory. It is a porous material that offers a large surface area and, due to the chemical nature of the Silica gel surface composed of silanol groups, makes they can form hydrogen bonds with polar compounds, such such as alcohols, terpenic alcohols, sesquiterpenic alcohols, aldehydes, terpenic aldehydes, phenols, carboxylic acids, Amides, amines.

Examples of essential oil to enrich include citrus essential oils such as orange ( Citrus sinensis ), lemon ( Citrus limonum ), tangerine ( Citrus reticulata ) and grapefruit ( Citrus paradisi ), as well as thyme oil ( Thymus vulgaris ), oregano oil ( Origanum vulgaris ), clove oil ( Syzygium aromaticum ), nutmeg oil ( Myristica fragrans ), cinnamon oil ( Cinnamomum zeylanicum ), bay oil ( Laurus nobilis ), peppermint oil ( Mentha x piperita ), valerian oil ( Valeriana officinalis ), citronella oil ( Cymbopogon nardos ), lavender oil ( Lavender angustifolia ), rose oil ( Rosa damascena ), Immortal oil ( Helicrysun stoechas ), rosemary oil ( Rosemarinus officianalis ), neem oil ( Azadirachta indica ), among others or mixtures thereof.

Once the essential oil has passed to enrich through the hydrophilic stationary phase, it is done passing a gas through said hydrophilic stationary phase (stage b), with the aim of eliminating traces of oil Essential not absorbed. Preferably, a refrigerant in a gaseous state such as nitrogen or 1,1,1,2 TFE. Said gas is passed through the stationary phase to a temperature between -18 ° C and 80 ° C, preferably between 10 ° C and 40 ° C

Next, the refrigerant is passed in liquid state through the hydrophilic stationary phase. The essential oil components absorbed in said phase hydrophilic stationary are eluted in said refrigerant, which is taken to a suitable pressure vessel.

Finally, said refrigerant is evaporated by expansion, thus separating from the oil components essential, that remain in liquid state without residue of refrigerant and are removed from the system. The refrigerant in state gas is compressed again under pressure to thus remain ready for a new cycle of the present procedure invention.

Advantageously, the essential oil enriched obtained according to the process of the present invention maintains the same color as the essential oil without enriching.

The present invention will be described in Below with more details in reference to an example of realization. This example, however, is not intended to limit the technical scope of the present invention.

Examples

Example one

Obtaining enriched lemon essential oil

10 kg of essential oil of lemon through a support containing 500 g of silica gel at a flow of 2 liters / h. Nitrogen was then passed gas through the silica gel bed for 10 min. Subsequently, 12 kg of 1,1,1,2-TFE in liquid state.

200 g of enriched oil 3 were obtained times in polar compounds.

Example 2

Obtaining lavender essential oil enriched in polar compounds

10 kg of lavender essential oil was passed through a support containing 1000 g of silica gel at a flow rate of 4 liters / h. Next, 1,1,1,2-TFE gas was passed through the silica gel bed for 10 min. Subsequently, 12 kg of 1,1,1,2-TFE were passed in the state
liquid.

350 g of lavender oil were obtained enriched 3 times in polar compounds.

While the invention has been described with respect to examples of preferred embodiments, these are not due consider limiting the invention, which will be defined by the broader interpretation of the following claims.

Claims (10)

1. Essential oil enrichment process in which a compression refrigeration cycle is used comprising the steps
from:

to)

do passing said essential oil through a stationary phase hydrophilic;

b)

do passing a gas through said stationary phase;

C)

elute the absorbed components by passing a refrigerant in form liquid through said hydrophilic stationary phase; Y

d)

evaporate said refrigerant.

2. Method according to claim 1, characterized in that said hydrophilic stationary phase is silica gel or alumina. 3. Method according to claim 1 or 2, characterized in that step a) is carried out in a laminar flow regime without stirring. Method according to any one of the preceding claims, characterized in that the essential oil to be enriched is an essential oil of citrus fruits such as orange ( Citrus sinensis ), lemon ( Citrus limonus ), tangerine ( Citrus reticulata ) and grapefruit ( Citrus paradisi ), Thyme oil ( Thymus vulgaris ), oregano oil ( Origanum vulgaris ), clove oil ( Syzygium aromaticum ), nutmeg oil ( Myristica fragrans ), cinnamon oil ( Cinnamomum zeylanicum ), bay oil ( Laurus nobilis ), el peppermint oil ( Mentha x piperita ), valerian oil ( Valeriana officinalis ), citronella oil ( Cymbopogon nardos ), lavender oil ( Lavender angustifolia ), rose oil ( Rosa damascena ), Immortal oil ( Helicrysun stoechas ), oil of rosemary ( Rosemarinus officianalis ), neem oil ( Azadirachta indica ), or mixtures thereof. 5. Method according to any of the preceding claims, characterized in that in stage b) a refrigerant is used in a gaseous state, such as 1,1,1,2-TFE or nitrogen. Method according to any of the preceding claims, characterized in that in step (b) the gas is passed through the stationary phase at a temperature between -18 ° C and 80 ° C, preferably between 10 ° C and 40 ° C. Method according to any one of the preceding claims, characterized in that the refrigerant used in stages c) and d) is a hydrochlorofluorohalides (HCFC) or hydrofluorohalide (HFC) type refrigerant that does not affect the ozone layer and is permitted by legislation. , such as R-123 (2,2-dichloro-1,1,1-trifluoroethane), R-124 (2-chloro, 1,1,1,2-tetrafluoroethane), or a mixture thereof. Method according to any of the preceding claims, characterized in that the refrigerant used in steps c) and d) is (1,1,1,2 tetrafluoroethane) when the product to be obtained is destined for feeding. 9. Procedure, according to any of the previous claims, wherein the essential oil enriched obtained maintains the same color as the essential oil without enriching 10. Procedure, according to any of the previous claims, wherein said stationary phase hydrophilic is contained in a suitable support to support high operating pressures, preferably up to 100 bar, more preferably up to 25 bar.