JP2547581B2 - Natural fat and oil processing method - Google Patents

Description

TECHNICAL FIELD The present invention relates to improvement of separation efficiency in a process of recovering a small amount of carotene contained in natural fats and oils.

2. Description of the Related Art Carotene has a wide range of uses as an edible colorant, a provitamin A substance, etc., and can be obtained by recovering what is contained in natural fats and oils. As a method for recovering carotene in natural fats and oils, the natural fats and oils are subjected to alcoholysis with a lower alcohol, and an oil phase containing carotene and containing a fatty acid lower alkyl ester as a main component is collected, and a hydrophilic solvent and water are added to the oil phase. Is mixed to precipitate carotene at an elevated temperature,
A method of extracting and separating and recovering a carotene concentrate (lower layer) containing carotene and a part of fatty acid lower alkyl ester and a hydrophilic phase (upper layer) containing most of fatty acid lower alkyl ester, hydrophilic solvent and water is recovered. It is known (Japanese Patent Laid-Open No. 61-115062). By cooling this upper layer, it is separated into an upper layer containing a hydrophilic solvent and water and a lower layer containing a fatty acid lower alkyl ester. The separated and recovered hydrophilic solvent and water are recycled to the carotene extraction step.

However, in this processing system, the upper layer and the lower layer were not separated promptly in the separation step, and there was a process problem.

That is, when the stationary separation method is adopted in the separation step, it is necessary to lengthen the residence time in the separation layer in order to complete the separation, and the apparatus becomes large. Further, when the centrifugal separation method is adopted, a large-sized centrifugal separator is required, which increases equipment costs.

Insufficient separation in the separation process after carotene extraction,
The carotene concentration efficiency decreases. Further, when separation failure occurs in the separation and recovery step of the hydrophilic solvent and water, the concentration of the lower fatty acid alkyl ester in the hydrophilic solvent and water to be recycled increases, affecting the carotene extraction step,
Systemically unfavorable.

OBJECT OF THE INVENTION It is an object of the present invention to improve the separation efficiency by a simple and compact operation in a method for treating natural fats and oils for extracting and recovering carotene.

Constitution of the Invention The method for treating natural fats and oils of the present invention comprises collecting an oil phase containing carotene and containing fatty acid lower alkyl ester as a main component, which is obtained by alcoholyzing a natural fat and oil containing carotene with a lower monoalcohol. Along with this, a hydrophilic solvent and water are mixed with this oil phase to precipitate carotene, and in the method for treating natural fats and oils in which the precipitated carotene is collected, the fatty acid lower alkyl ester in which the precipitate is precipitated, the hydrophilic solvent and water are precipitated. The mixture is allowed to pass through an agglomerate composed of a fibrous filler, and then the precipitate and the residual liquid are separated.

Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings.

As an object to be treated in the present invention, an oil phase obtained by alcoholysis of a carotene-containing natural fat or oil such as palm oil is used. By adding lower alcohols such as methanol and ethanol to carotene-containing natural fats and oils, glycerides in the natural fats and oils are subjected to alcoholysis and converted into glycerin and lower alkyl esters of higher fatty acids. Carotene is contained in an oil phase containing fatty acid lower alkyl ester as a main component, and this oil phase is collected by separating it from glycerin by an appropriate means such as static separation or centrifugation.

A hydrophilic solvent and water are mixed with this oil phase to precipitate and separate carotene to obtain a carotene concentrate. As shown in FIG. 1, the oil phase is mixed with a hydrophilic solvent and water, and the heat exchanger 11
At elevated temperature, the carotene is precipitated at 30 to 120 ° C.,
Extract. At this time, the carotene concentrated phase exists as fine oil droplets (for example, a diameter of about 1 to 10 μm), and the remaining lower fatty acid lower alkyl exists in a dissolved state in the hydrophilic phase. When this is statically separated, the oil droplets are aggregated and separated, but it takes a long time for the minute oil droplets to be separated. In the present invention, the extract containing the oil droplets is passed through the aggregating part filled with the fibrous material. The oil droplets in the extract that come out from the agglomerate grow and become large, for example, grow to a diameter of about 5 to 10 mm. When oil droplets are adsorbed and aggregated on the fiber surface, a separated oil layer is generated in the fibrous packing, and when the dispersed minute oil droplets pass, coalescence and aggregation of oil droplets are promoted. It is considered that the oil droplet diameter grows.

As the fibrous material used here, a fibrous material that is easily wetted by a fatty acid lower monoalkyl ester is used, and a material that can include a large amount of a fatty acid lower alcohol ester in a yarn thread is preferably used.

As specific fibrous materials, polyvinyl chloride, polyvinylidene chloride, promix fiber, nylon, polyester, polyethylene, polypropylene, glass wool can be preferably used.

There are no particular restrictions on the wire diameter of the fibrous filler, the packing density, the liquid passing speed of the agglomeration part, etc., but a finer wire diameter is preferable because the contact area between the fiber and the oil droplet per unit volume increases.
The packing density is preferably 0.05 to 0.3 g / cm ³ , and the liquid passing speed through the agglomerate is preferably 30 to 150 cm / min in linear velocity.

The extract liquid, which has passed through the aggregating section and where the precipitated oil droplets have been coalesced and agglomerated, is guided to the separation section and statically separated (separation step I).

The oil droplets are aggregating and growing, so separation proceeds rapidly,
Even a small separation device separates into an upper layer and a lower layer in a relatively short time. The lower layer contains carotene and a part of fatty acid lower alkyl ester, and the carotene-containing concentrate is recovered by fractionating this.

The top layer contains most of the fatty acid lower alkyl esters, hydrophilic solvent and water. When the recovered upper layer is cooled by the heat exchanger 13 and adjusted to, for example, about 10 to 30 ° C., a decarotene fatty acid lower alkyl ester layer is deposited, and for example, 1 to
It becomes a minute oil droplet of about 10 μm.

In this case as well, as in the above separating step I, a large load is applied when the separation is performed as it is. Therefore, it is desirable to pass through the aggregating portion as described above. Preferable aspects, specific examples, etc. of the aggregating portion are the same as those already described in the separation step I.

When passing through the aggregating part, oil droplets of fatty acid lower alkyl ester aggregate and coalesce, and typically grow up to about 5 to 10 mm.

The treatment liquid that has passed through the agglomeration section and has grown in oil drop size is guided to the separation section and statically separated (separation step II).

Here, as in the separation step I, the oil droplets are agglomerated, and even a small-sized separation device separates into an upper layer and a lower layer in a relatively short time. The decarotated lower fatty acid ester is recovered as the lower layer. From the upper layer, the hydrophilic solvent and water are recovered and recycled as an oil phase extractant.

EFFECTS OF THE INVENTION According to the present invention, when natural fats and oils are treated and carotene is deposited and separated, the fibrous filler is passed through and treated prior to this separation, whereby the precipitated fine oil droplets aggregate and combine. First, the particle size becomes large, and the separation can be performed by a simple operation. Therefore, the residence time of the extract in the separator is short, and a compact separator can be used, which is suitable as an industrial natural fat / oil processing method.

Example 1 Crude palm oil containing 610 ppm of carotene was mixed with methanol and caustic soda at a ratio of crude palm oil / methanol / caustic soda = 73.7 / 25.8 / 0.5 (% by weight) to carry out a methyl esterification reaction. Let it be done. The produced ester layer was collected, washed with 1/5 volume of crude palm oil, and then dehydrated by a conventional method.

Next, an aqueous methanol solution containing 11.5% by weight of water was mixed in an amount 6.5 times that of the ester layer, and the temperature was raised to 80 ° C. for extraction treatment. In this mixed solution, a 4.1 wt% carotene concentrated layer was present as free oil droplets, and the remaining ester was present in a dissolved state in the methanol / water layer. This mixed solution was continuously supplied to the aggregating part filled with polyvinyl chloride fiber having a wire diameter of 16 μm at a packing density of 0.12 g / cm ³ , and then introduced into the separating part and allowed to stand and separate (separation step I). A carotene concentrate having a carotene concentration of 1880 ppm was obtained from the lower layer of the separation part. Free oil droplets in the upper layer of the separation part decreased to 0.12% by weight (separation degree 97.0%). The linear velocity of the mixed solution supplied to the aggregating section was 100 cm / min, and the total liquid residence time in the aggregating section and the separating section was 30 seconds.

Further, when the recovered upper layer was cooled to 20 ° C., oil droplets were deposited, 7.3% by weight of oil droplets were freely present, and 2.0% by weight of ester was present in a dissolved state. This upper layer was supplied to the aggregating part filled with polyvinyl chloride fibers in the same manner as above, and then introduced into the separating part and allowed to stand and separate (separation step II). From the lower layer of this separation part, decarotated methyl ester having a carotene concentration of 80 ppm was obtained. Free oil droplets in the upper layer of the separation part was 0.3% (separation degree 96.0%). The supply linear velocity to the agglomeration section and the total residence time of the agglomeration section and the separation section were 98 cm / min and 30 seconds, respectively.

Comparative Example 1 When the polyvinyl chloride fibers filled in the agglomerated part were removed and the same operation as in Example 1 was performed, the separation degrees in separation steps I and II were 37.0% and 34.3%, respectively.

Example 2 0.15 / cm ³ of polyvinylidene chloride having a wire diameter of 40 μm was applied to the agglomerated portion.
When the same procedure as in Example 1 was carried out, the separation degrees in separation steps I and II were 96.0% and 95.5%, respectively.

However, the linear feed rate to the agglomeration part was 50 cm / min, and the residence time was 1 minute.

Example 3 When glass wool having a wire diameter of 7 μm was filled in the agglomerated portion and operated under the same conditions as in Example 2, the separation degrees in separation steps I and II were 94.2% and 95.0%, respectively.

Example 4 When the same operation as in Example 1 was performed using the fillers made of various fiber materials shown in Table 1 below, the degree of separation in the separation steps I and II was as shown in Table 1. It was

[Brief description of drawings]

 FIG. 1 is a process diagram showing an embodiment of the present invention. 11,13 …… Heat exchanger

Claims (1)

(57) [Claims] 1. A caroten-containing natural fat and oil obtained by alcoholysis with a lower monoalcohol, and an oil phase containing carotene and containing a fatty acid lower alkyl ester as a main component is collected and hydrophilic to this oil phase. In a method for treating natural fats and oils by mixing a solvent and water to precipitate carotene and collecting the precipitated carotene, a mixture of the fatty acid lower alkyl ester in which the precipitate is deposited, the hydrophilic solvent and water is removed from the fibrous filler. The method for treating natural fats and oils, which comprises separating the precipitate and the residual liquid after passing through the agglomerating part.