JP3261764B2 - Method for producing sucrose fatty acid ester plate - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a sucrose fatty acid ester (hereinafter abbreviated as SE) plate. More specifically, the present invention relates to a method for concentrating an SE solution into an SE melt, and then cooling and solidifying the same to produce a plate.

[0002]

2. Description of the Related Art SE has excellent interfacial performance, good biodegradability and high safety, and is conventionally used as an additive for foods, cosmetics, pharmaceuticals, kitchen detergents, feeds, resins, and the like. In the chemical industry, it is used as an auxiliary in a reaction system such as a polymerization reaction and an oxidation reaction, and is a very useful compound.

As a conventional SE production method, a method of reacting sucrose with a fatty acid alkyl ester in an organic solvent such as dimethylformamide or dimethyl sulfoxide in the presence of an alkali catalyst, using water without using an organic solvent. After the sucrose is melt-mixed with the fatty acid soap, a method is known in which a fatty acid alkyl ester is reacted in the presence of an alkali catalyst, and a so-called bio-method in which sucrose and a fatty acid are directly reacted in the presence of a specific enzyme. Have been.

[0004] SE produced by these methods is commercialized through post-treatment and purification steps, and the final product is in the form of paste, powder, or the like. The paste can be produced by appropriately concentrating a dilute solution of SE. As a method for producing a powder, a spray drying method in which a dilute solution of SE is concentrated and dried is known (JP-A-2-117691, JP-A-2-134391, and JP-A-2-40390).

[0005]

The spray drying method has the advantage that the process is simple, but the heat source cost is large, the solvent is not sufficiently cut off, and it tends to cause the solidification of the powdered product. As a method other than spray drying, a method in which the concentrated SE is once cooled and solidified to form pellets or flakes and then pulverized may be considered, but no industrially satisfactory method has yet been proposed.

[0006]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies in view of the above circumstances, and as a result, have concentrated the SE solution efficiently to sufficiently reduce the solvent content. The present inventors have found that by cooling and solidifying, it is possible to obtain an SE plate-like body which hardly solidifies even when pulverized and can give a good SE powder, and thus completed the present invention.

That is, the gist of the present invention is to concentrate a solution of a sucrose fatty acid ester to a solvent content of 5% or less using a thin film evaporator at a temperature not lower than the melting temperature of the sucrose fatty acid ester,
The method for producing a sucrose fatty acid ester plate-like body characterized in that the obtained molten sucrose fatty acid ester is sandwiched between a rotating drum having a cooling medium therein and an endless belt and cooled and solidified in a plate shape. is there.

Hereinafter, the present invention will be described in detail. SE in the present invention has 6 to 30 carbon atoms, preferably 12 carbon atoms.
~ 22 saturated or unsaturated fatty acids (e.g. caproic acid,
Saturated fatty acids such as capric acid, lauric acid, myristic acid, palmitic acid, stearic acid and behenic acid; unsaturated fatty acids such as linoleic acid, oleic acid, linoleic acid, erucic acid and ricinoleic acid) and having 1 to 6 carbon atoms It is produced by transesterifying an ester with a lower alcohol (eg, methanol, ethanol, propanol, butanol, etc.) and sucrose.

The solvent for the SE solution is usually an organic solvent dissolving SE such as hexane, n-butanol, isobutanol, methyl ethyl ketone, methyl isobutyl ketone, and water, and these solvents can be used alone or as a mixture. . Water is particularly preferred when producing SE for applications such as food, cosmetics, pharmaceuticals, feed and the like. The concentration of SE in the SE solution in the present invention is usually 1 to 90% by weight, preferably 20 to 60% by weight.

The concentration in the present invention can be used in combination with a preconcentration by a distillation column or evaporation and a thin film evaporator. Such a thin film evaporator is usually a rising thin film evaporator,
A falling film type, a horizontal thin film type, and a type in which the above-described various types and a rotating blade are rotated in a heating tube are employed. Preferably, a combination of a falling thin film type and a type of rotating a rotary blade in a heating tube, and a combination of a horizontal thin film type evaporation type and a type of rotating a rotary blade in a heating tube are used. A plurality of thin film evaporators can be used by connecting them in series.

The concentration in the present invention is carried out at a temperature of 40 to 150.
° C, pressure 10 ~ 760mmHg, preferably temperature 70 ~
The process is performed at 120 ° C. and a pressure of 50 to 100 mmHg until the solvent content becomes 5% or less, preferably 1.5% or less. When the content of the solvent is 5% or more, when the cooled and solidified SE plate is further pulverized, it causes caking of the obtained powder.

In the present invention, the cooling and solidification is performed by using a drum-type cooler and bringing molten SE into contact with the endless belt for a certain period of time between the rotating drum cooled by supplying a refrigerant therein and the endless belt. (See Japanese Patent Publication No. 2-9273.) The drum type has a small installation area and is easily sealed, so that dust and the like can be prevented from being mixed. In addition, cooling efficiency is good,
Deformation due to heat shrinkage can be prevented. In this respect, the drum type cooler is capable of melting molten S on a steel belt conveyor.
This is very superior to a conventional device in which E is allowed to flow and stay for a certain period of time to cool.

The rotating drum and the endless belt of the drum type cooler are usually made of iron.
Stainless steel materials are preferred. The surface of the rotating drum can be used without surface finishing, but surface finishing is preferable because a high quality product can be obtained. Cooling of the rotating drum is performed by supplying a cooling medium from the inside of the rotating drum.
Refrigerant temperature requires cooling required to solidify SE in a molten state, and is usually −20 to 50 ° C., preferably −10 to 10 ° C.
Use a refrigerant in the range of 20 ° C.

[0014] The molten SE is mainly cooled by the refrigerant in the rotating drum, and the temperature of the molten SE after cooling is lower than the melting point of SE, and is usually cooled to 10 to 50 ° C. Solidified S
In order to prevent the dew condensation of E, it is usually preferable to introduce a dehumidified gas into the drum-type cooling device. At this time, it is preferable that the entire drum-type cooling device is set in an enclosure having a closed structure, and dry air, dry nitrogen, and the like are circulated in the enclosure.

The material of the endless belt of the drum type cooler in the present invention is not limited, but can be usually selected from iron, stainless steel, copper, glass fiber, polymer material and the like. In the case of SE for products such as foods and pharmaceuticals, a material obtained by coating glass wool with Teflon is preferable. Although the thickness of the SE solidified from the molten SE into a plate shape by the endless belt and the drum of the drum type cooler in the present invention is not particularly limited, it is usually preferably 0.1 to 10 mm. Although the plate-like SE in the present invention is not limited thereafter, continuous pulverization in a drum-type cooler is efficient as an industrial production method.

[0016]

The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples unless it exceeds the gist. Example 1 A horizontal thin film containing an aqueous solution containing 51.0% by weight of palmitic acid SE (monoester content: 80%, equivalent to Ryoto Sugar Ester P-1670) produced by a reaction method using dimethyl sulfoxide (DMSO) as a solvent. Evaporator (using horizontal control from Hitachi, Ltd. Heat transfer area is 14m ² )
At a rate of 816 kg / hour. Evaporation condition is temperature 100
° C and a pressure of 80 mmHg. The solvent (water) content in SE palmitate discharged from the horizontal thin film evaporator is 0.62.
%Met. Next, 419 kg / mol of the palmitic acid SE in a molten state (about 100 ° C.) discharged from the horizontal thin film evaporator was used.
Every hour, it was introduced into a drum-type cooler (Model DC-1500S21, manufactured by Mitsubishi Kasei Engineering Corporation).

The material of the endless belt was glass wool coated with Teflon, and the refrigerant in the rotating drum was supplied at 0 ° C. The thickness of the solidified SE is 3mm
It was adjusted to become. The rotation speed of the rotating drum was set at 0.4 rpm. Room temperature dry air was supplied into the sealed drum cooler device. The temperature of the SE solidified into a plate under the above conditions was 30 ° C. The shape of the obtained plate-like body after being pulverized by a coarse pulverizer attached to a drum-type cooler was an irregular flake having a length and width of about 2 to 3 cm. This flake-like palmitic acid SE was finely pulverized with an impact type fine pulverizer manufactured by Hosokawa Micron Co., Ltd. to obtain a white powder having an average particle diameter of 32 μm and a water content of 0.83%. Then, the white powder was stored in a mayonnaise bottle at 35 ° C.
After the lapse of time, no caking occurred.

Example 2 An SE plate having a thickness of 3 mm and a temperature of 30 ° C. was obtained by cooling and solidifying in the same manner as in Example 1 by using a palmitic acid SE having a water content of 1.10% from a horizontal thin film evaporator. Was. Then, a water content of 1.24 was obtained by coarse pulverization and fine pulverization in the same manner as in Example 1.
% Of SE white powder was obtained. At 35 ° C., no consolidation occurred for 110 hours or more.

Example 3 Melt-state stearic acid SE (equivalent to Ryoto Sugar Ester S-117) with a water content of 0.55% discharged from a horizontal thin film evaporator was supplied to a drum type cooler at 550 kg / hour. Except having performed, it carried out similarly to Example 1. As a result, the temperature of the SE solidified in a plate shape was 30 ° C., and the thickness of the plate was 3 mm. Further, coarse pulverization and fine pulverization were carried out in the same manner as in Example 1, and the storage stability at 35 ° C. was very good.

EXAMPLE 4 A molten state of stearic acid SE (equivalent to Ryoto Sugar Ester S-770) having a water content of 2.73% discharged from a horizontal thin film evaporator was introduced into a drum type cooler at a rate of 410 kg / hour. Other than that, it carried out similarly to Example 1. As a result, the temperature of the SE solidified in a plate shape was 30 ° C. and the plate thickness was 3
mm. Subsequently, pulverization was carried out, and when storage stability was observed, caking did not occur even after 1000 hours at 35 ° C.

Comparative Example 1 SE of palmitic acid SE having a water content of 5.2% discharged from a horizontal thin film evaporator was cooled and solidified in the same manner as in Example 1. Subsequently, pulverization was performed, but the resulting powder immediately solidified at 35 ° C. Comparative Example 2 The same procedure as in Example 3 was carried out to cool and solidify SE of stearic acid SE having a water content of 5.1% discharged from the horizontal thin film evaporator. However, following grinding, the white powder immediately solidified.

[0022]

As described above, the SE melt can be continuously formed into a plate by a compact apparatus. The plate is crushed and SE
It can be used as a powder.

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor, Tsunemi Arita 1 Tohocho, Yokkaichi-shi, Mie, Mitsubishi Kasei Co., Ltd. (72) Inventor Yukio Kasori 1-Tohocho, Yokkaichi, Mie, Japan Yokkaichi, Mitsubishi Inside the factory (56) References JP-B-58-4038 (JP, B2) (58) Fields investigated (Int. Cl. ⁷ , DB name) C07H 13/06

Claims (3)

(57) [Claims] 1. A solution of a sucrose fatty acid ester is concentrated to a solvent content of 5% or less using a thin film evaporator at a temperature not lower than the melting temperature of the sucrose fatty acid ester, and the obtained molten sucrose fatty acid ester is internally contained. A method for producing a sucrose fatty acid ester plate, wherein the plate is cooled and solidified in a plate shape between a rotary drum having a cooling medium and an endless belt. 2. An atmosphere for cooling and solidification is sealed by a partition,
2. The method according to claim 1, wherein a dry gas is circulated in each closed space. 3. A water content of 1.5% using a thin film evaporator.
2. The method according to claim 1, wherein a molten sucrose fatty acid ester concentrated to the following level is used.