JPH0253896A - Purification of jojoba oil - Google Patents

Abstract

PURPOSE:To obtain a colorless, transparent and virtually oderless purified oil, optimum as a cosmetic base and useful as a medical raw material by treating a low-boiling hydrocarbon solution of jojoba oil with a column packed with a cation exchange resin to be used for non-aqueous solution. CONSTITUTION:Firstly, jojoba oil is dissolved in a low-boiling hydrocarbon such as m-pentane, n-hexane or n-heptane so as to be 5-95wt.% in concentration. Thence, the resultant solution is treated through a column packed with a strongly acidic cation exchange resin having pref. sulfonic acid group to be used for non-aqueous solution and an adsorbent consisting of activated alumina or activated carbon at the weight ratio pref. 1:(0.5-3), thus obtaining the objective purified product.

Description

[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a method for refining jojoba oil, which is a colorless and transparent oil that is particularly suitable for use as a base for cosmetics and can also be used as a raw material for pharmaceuticals. The present invention relates to a method for obtaining an almost odorless refined oil.

[Conventional technology]

In general, oils and fats have been purified by a decolorization method using an adsorbent such as activated carbon or activated clay, or a deodorization method by steam injection. In addition, oils and fats are treated with alkali, the precipitated grains are hydrolyzed by acid aqueous solution treatment, and further purification methods such as steam distillation (Japanese Unexamined Patent Publication No. 73793/1983), under reduced pressure, at a specific temperature and time, and with steam A method of performing steam distillation with a blowing amount (Japanese Patent Application Laid-Open No. 61-23698), a method of using various granular adsorbents to remove free fatty acids and phosphorus compounds from vegetable oils and fats (West German Patent Publication No. 2.226.293) issue specification),
Method for removing free fatty acids in frying oil by aluminum hydroxide gel (oil chemistry.

23.296 (1974)), a method of decolorizing and deodorizing a hexane solution of soybean oil by passing it through a polyacrylonitrile (IRIS 3042) membrane run, ultrafiltering the liquid through a silica gel column, and treating it with steam and clay ( West German Patent Publication No. 2,651.761) is known. Furthermore, as a purification method using an ion exchange resin, a method of treating crude oils and fats with a strongly basic anion exchange resin having a quaternary ammonium hydroxide group to remove coloring components and free fatty acids (U.S. Pat. No. 2,771
．． No. 480 [i-], a method of decolorizing and removing free fatty acids using a sulfonated phenol-aldehyde resin (U.S. Pat. No. 2,863,890), and the like.

[Problem to be solved by the invention]

When fats and oils are used as a base for cosmetics, it is undesirable if the fats and oils are colored, as this may lead to deterioration in the quality of the products in which they are blended, so oils and fats that are colorless, transparent, and have a mild odor are required.

Currently, jojoba oil is obtained through clay treatment, molecular distillation, and deodorization to obtain refined oil, but there is a need to further improve the quality of refined oil.

The purpose of the present invention is to provide a method for obtaining purified jojoba oil that is colorless and transparent and has a mild odor.As a result of extensive research, the following method was discovered.

That is, the present invention is a method for refining jojoba oil, which is characterized by treating a low-boiling hydrocarbon solution of jojoba oil in a column packed with a cation exchange resin for non-aqueous solutions and activated alumina or activated carbon.

Specific examples of low-boiling hydrocarbons used as eluents for dissolving jojoba oil in the present invention include n-pentane,
They are n-hexane and n-hephthanato, and the concentration of jojoba oil dissolved in these solvents is 5 to 90% by weight. However, in view of the viscosity of the solution, the optimum concentration for allowing the solution to pass smoothly through the column filled with the ion exchange resin and the auxiliary column filled with the adsorbent is 5 to 70% by weight. In addition, ion exchange resins suitable for use in non-aqueous solutions are highly acidic cation exchange resins with sulfonic acid groups (
Acid type) is preferable, and commercially available products include, for example, Noanhar +) manufactured by Hallom and Haas, X) (Amber
list) 15 are listed.

On the other hand, activated alumina or activated carbon is used as the adsorbent. Many activated aluminas are commercially available in basic and acidic types, and they also come in powder and granule forms. Among them, granular ones are easier to use. As a commercially available product, for example, Sumitomo Alumina KG manufactured by Sumitomo Chemical Co., Ltd.
O-1442 (granular), KGD-1442 (granular), KCG-30 (powder) and West German I CN Biome
A1umjnaWoe1m A-8u manufactured by dicals
There is per I. On the other hand, as for activated carbon, relatively small particles are easy to use, such as Wako Pure Chemical Industries Ltd.
Made of activated carbon (297 μ or more max 4 (1% +
There are 297μ to 63μ m1n50%).

The cation exchange resin for non-aqueous solutions and the adsorbent may be mixed together and packed in a column in the form of a mixed bed, or a single column may be prepared and used by connecting them in series.

In the former case, the mixing ratio of the adsorbent to the cation exchange resin for non-aqueous solutions is 10 to 300 to 30% by weight. In the latter case, each column is filled with adsorbent in the same ratio as above.

The ratio of the amount of jojoba oil to be purified to the amount of ion exchange resin and adsorbent used for the treatment is preferably 1:0.5 to 3 (weight ratio).

Column Chroma Dog 2 Fee is carried out at room temperature and normal pressure, and the amount of eluent is suitably 10 to 15 times the amount of jojoba oil used for the treatment. The eluate is first collected by distilling the solvent at normal pressure, and then the remaining small amount of solvent is distilled under reduced pressure (approximately 20 m
mHg), by distilling it off at a temperature of 60° C. or lower, a purified jojoba oil that is transparent, colorless, and has a mild odor can be obtained. If you want to obtain an odorless product, you can purify it using a normal deodorizing method.

[Effect]

Generally, when special fats and oils such as jojoba oil are treated with conventional decolorization methods, it is possible to remove the color from pale yellow, but beyond that it is difficult. In the reaction with a cation exchange resin for non-aqueous solutions, nitrogen-containing compounds with weak cationic properties are selectively adsorbed and removed, and pigment components that cannot be removed are treated with an active column that is mixed into an auxiliary column or a mixed bed column. Coloring components can be almost completely removed by adsorption to alumina.

〔Effect of the invention〕

The refined jojoba oil obtained by the present invention not only has a lower free fatty acid content than refined oil obtained by conventional methods, but also has significantly improved hue and odor, and also has less fluctuation in composition due to selective adsorption onto the column. Almost unrecognized. ! Since it is colorless and transparent and has a mild odor, it is suitable for use as a base for cosmetics, as well as as a raw material for the pharmaceutical industry and the oil and fat chemical industry.

〔Example〕

Next, the present invention will be explained in detail with reference to Examples.

Example 1 Jojoba crude oil 502 was dissolved in n-hexane 30d, and an acid type cation exchange resin for non-aqueous solutions (Amblyst '15.
The weight ratio of Rohm and Haas M> and activated alumina (Sumitomo Alumina KGO-1442° granules) is 80:2.
The mixture was injected into a glass column (30 mmσ x 60 cm) packed with 8Of and adsorbed.

Subsequently, the eluent was eluted with about 500 nm of n-hexane, and the eluate was distilled at normal pressure and then further distilled under reduced pressure (20 Tmnnng).
At 50°C, a small amount of remaining eluent was distilled off to 46°8? obtained refined oil. The quality of the obtained refined oil is shown in Table 1.

Example 2 501 jojoba crude oil was thoroughly mixed with 25 mff1 of n-hebutane, and the cation exchange resin for non-aqueous solutions used in Example 1 and activated alumina (Sumitomo Alumina KCG-30, powder) were mixed in a weight ratio of 90:10. 8OL mixed in proportion? The mixture was injected into a glass column (30wn f5x60m) packed with 4601 for adsorption, and then eluted with about 500 g of n-hebutane.The same procedure as in Example 1 was repeated to obtain purified oil 4601. The quality of the obtained refined oil is shown in Table 1.

Example 3 50 g of jojoba crude oil was dissolved in 70 M of n-pentane, and the cation exchange resin for non-aqueous solutions used in Example 1 and activated alumina (Alum manufactured by ICN Btomedicals, West Germany) were dissolved.
Ina Woelm A-8upper I) mixed at a weight ratio of 70:30 was injected into a glass column (30 amρ x 60 tyn) packed with 802 for adsorption, and then eluted with about 500 n-pentane. Thereafter, the same procedure as in Example 1 was carried out to obtain 45.2 f refined oil.

The quality of the obtained refined oil is shown in Table 1.

Example 4 40 g of jojoba crude oil was dissolved in 40 d of n-hexane, and the cation exchange resin for non-aqueous solutions used in Example 1 and granular activated carbon (activated carbon manufactured by Wako Pure Chemical Industries Ltd., for chromatography) were added in weight ratio. A mixture of 601 in a ratio of 85:15 was injected into a glass column (30wnβx60cm) for adsorption, and then eluted with about 400d of n-hexane. of refined oil was obtained.

The quality of the obtained refined oil is shown in Table 1.

Example 5 A glass column (30 mm x 60 ports) packed with the cation exchange resin 602 for non-aqueous solutions used in Example 1 and a glass column (30 mm x 3 o cm) packed with 20 g of granular activated alumina (used in Example 1) ) are connected in series, and then decorated with 4019 jojoba crude oil dissolved in 20-hexane.

Subsequently, about 400 d of n-hexane was added as an eluent, and the eluent was used in the same manner as in Example 1 to obtain 358 ml of n-hexane. of refined oil was obtained. The quality of the obtained refined oil is shown in Table 1.

Comparative Example 1 1.0% by weight of activated clay and 0% by weight of jojoba crude oil 1002
．． 2% by weight of activated carbon was added and decolorization was carried out at 100° C. for 30 minutes in a conventional manner. The obtained decolorized oil was further heated at 3 to 5 mmHg +190°C while blowing in water vapor.
After time deodorization, a refined oil of 96.9 SF was obtained. The quality of the obtained refined oil is shown in Table 1.

Comparative Example 2 Jojoba crude oil 509 was dissolved in 50 m/n-hexane and injected into a glass column (30 mm B Eluted with n-hexane. Thereafter, the same procedure as in Example 1 was carried out to obtain a refined oil of 46°91. The quality of the refined oil obtained is shown in Table 1.

Comparative Example 3 A glass column (30 mm 8 x 60 cm) was prepared by dissolving 30 g of jojoba crude oil in n-hexane 301 and filling it with activated alumina (Jubishi Alumina KCG-30° powder) 802.
Then, using about 300 d of n-hexane as an eluent, the procedure was repeated in the same manner as in Example 1 to obtain 19.7 g of purified oil. Table 1 shows the quality of the refined oil obtained.

Comparative Example 4 3 t of jojoba crude oil was dissolved in 30 d of n-hexane, and a strongly acidic cation exchange resin for general aqueous solutions (Amberlite (A
amberlite) I R120B, manufactured by Rohm and Haas, USA) 502 glass column (
30wn0 x 60 gm), then about 500
eluted with n-hexane. Thereafter, the same procedure as in Example 1 was carried out to obtain a refined oil of 28.2 f.

Table 1 shows the quality.

As is clear from the results in Table 1, the purification method using a combination of the cation exchange resin for non-aqueous solutions and activated alumina or activated carbon of the present invention is superior to the treatment using these alone or to other purification methods. It can be seen that a refined oil of high quality is obtained with excellent color, color and odor.

Patent applicant: NOF Corporation

Claims (1)

[Claims] (1) A method for refining jojoba oil, which comprises treating a low-boiling hydrocarbon solution of jojoba oil in a column packed with a cation exchange resin for non-aqueous solutions and activated alumina or activated carbon.