JPH06200287A - Method for purifying natural crude wax - Google Patents

Abstract

PURPOSE:To effectively remove unnecessary ingredients from a natural crude wax by adding a given amount of a solvent to the wax, heating the mixture to around the melting point of the wax, removing the solvent-insoluble matter, further adding the solvent to the solution, cooling it to precipitate a solid matter, and conducting solid-liquid separation so that the wax recovered has a given solvent content. CONSTITUTION:A solvent (e.g. a 1-4C alcohol) is added to a crude wax (e.g. one obtained from sugar cane) in a wax to solvent ratio of 1:(3-20) by weight. The mixture is heated to a temp. in the range of [melting point of the wax] + or -20 deg.C to dissolve the wax. The resulting solvent-insoluble matter is removed by solid-liquid separation at such a temp. The solvent amount is then regulated so that the wax to solvent ratio becomes 1:(3-30) by weight. The resulting mixture is heated to a temp. in the range of [melting point of the wax] + or -20>=C and cooled to -10 deg.C to 40 deg.C to precipitate a solid matter. The solid is separated from the liquid with a centrifugal separator, etc., so that the solvent content of the solid becomes 50-90%. The solvent is removed from the resulting wax in solution or solid state.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a method for purifying natural crude wax. More specifically, it relates to a method for purifying a natural crude wax for refining the natural crude wax with a solvent to obtain a wax material preferable in various fields of application.

[0002]

2. Description of the Related Art Conventionally, as a method for purifying a natural crude wax, a natural crude wax is dissolved in a solvent and filtered to remove a resin component contained in the natural crude wax (JP-A-2-2797).
94), the crude wax is once dissolved in an organic solvent and then cooled to precipitate a wax component, which is simply filtered, and the solvent is separated and removed by distillation of the filtered wax component (JP-A-2-150496). Gazette) and the like, and has been applied to carnauba wax, candelilla wax and the like, which are characteristic among natural waxes.

[0003]

However, it is difficult to sufficiently remove the impurities contained in various natural crude waxes by the above-mentioned simple filtration method.
Therefore, the same purification process had to be repeated multiple times. However, since the composition of the natural crude wax is not constant, it is difficult to reduce the amount of unnecessary components contained to a certain value or less simply by dissolving it in a solvent and performing a precipitation operation or a filtration operation. Therefore, a uniform wax cannot be obtained by the above method, and there are problems in the recovery rate and the quality of the product.

[0004]

In view of such circumstances, the inventors of the present invention have been eager to identify harmful components that make the properties of the refined wax unstable during the refining process of the natural crude wax and to effectively remove them. As a result of repeated examination,
It was found that unnecessary components are resinous components contained in natural crude wax, glycerides, free unsaturated fatty acids, free sterols, and sterol ester components in which these fatty acids and sterols are bound, and The inventors have found that the unnecessary components can be effectively removed by combining specific steps, and have established a method for industrially producing a homogeneous natural wax, thus completing the present invention. That is, the method for purifying a natural crude wax of the present invention comprises an arbitrary step (a) and step (b) in the order, and the following step (c) to be performed thereafter. Step (a): The weight ratio of wax component to solvent is 1: 3 to 2
The wax component is dissolved by heating the mixture of 0 to a temperature range of 20 ° C. above and below the melting point of the wax, and the solvent-insoluble component is separated and removed from the solution by a solid-liquid separation operation while maintaining the temperature range. Step, Step (b): Weight ratio of wax component to solvent is 1: 3 to 3
The wax content is dissolved by heating the mixture of 0 to a temperature range of 20 ° C. above and below the melting point of the wax, and then the solid content of the wax is precipitated by cooling, whereby the solvent content in the solid content of the wax is reduced. A step of separating and recovering the wax solid content by a solid-liquid separation operation so as to be 50 to 90%, and a step (c): Among the steps (a) and (b),
A step of obtaining a purified wax by removing the solvent from the wax solution or the solid wax content obtained from the subsequent step.

The present invention will be further described below. First, the unnecessary components in the natural crude wax will be described. These are composed of the resinous component, glycerides, free unsaturated fatty acid component, free sterol component, and sterol ester component in which these fatty acids and sterols are bonded as described above, and prevent the crystallization of the wax to increase the hardness. Spoil. Further, among the above substances, one having a low melting point causes a decrease in the melting point of the whole wax. A component whose structure itself is unstable with respect to heat or an oxidizing atmosphere, such as one containing an unsaturated bond, causes the instability of the wax. The refining method of the natural crude wax of the present invention can be preferably applied to any natural crude wax regardless of plant type or animal type. For example, there are crude waxes such as sugar cane wax, bees wax, rice wax, carnauba wax and candelilla wax which are naturally produced and need to be refined. The wax in which the method of the present invention is particularly preferably adopted is a vegetable wax, more preferably a crude wax from sugar cane.

Here, a typical production method of sugar cane crude wax is shown. When the sugar juice squeezed and squeezed out of the sugar cane is allowed to stand in the raw sugar production process, a suspended substance mainly composed of fiber components and fats and oils floats above the juice. The filter cake obtained by separating this by filtration is dried,
Get a dry cake. Extraction is performed on this dried cake using a light organic solvent such as a hydrocarbon as an extraction solvent.
Immediately after the extraction is completed, filtration is carried out immediately to separate and remove the filtration residue. The filtrate is allowed to stand, the lower aqueous layer is separated, the solvent layer is distilled, and the solvent is removed to obtain crude sugar cane wax. Further, a crude sugar cane wax obtained by scraping off the stem surface of sugar cane and extracting with a hot water bath or an organic solvent can also be the object of purification. In addition, the refining method of the present invention can be applied to any natural crude wax that requires refining.

<Step (a)> In the step (a) of the method for purifying a natural crude wax of the present invention, 3 to 20 times by weight of a solvent is added to the raw material wax to be supplied, and the temperature is above and below the melting point of the wax at 20 ° C. The wax component is dissolved by heating to the internal temperature, and the solvent-insoluble component is removed by the solid-liquid separation operation while maintaining the same temperature. In order to effectively remove the solvent-insoluble matter in the wax, it is essential that the amount of the solvent is 3 to 20 times the weight of the raw wax.
If the amount of the solvent is less than 3 times by weight, the solid content cannot be effectively separated, and if the amount of the solvent is more than 20 times, no significant effect is exerted, which is economically disadvantageous. Practically, preferable results can be obtained by removing the insoluble matter using a solvent in an amount of 5 to 10 times the weight of the raw wax. In addition,
When the wax to be supplied contains a solvent, the amount of the solvent to be added is determined in consideration of the contained solvent. That is, when the amount of the solvent is insufficient, it is added separately, and when it is excessive, the amount of the solvent is adjusted to an appropriate amount by an appropriate method, such as distillation, and used.

Further, in the step (a), when the wax component is dissolved in the solvent, the temperature is set above and below the melting point of the wax.
Keep in the 0 ° C range. As long as the wax component is dissolved in the above temperature range, the wax component can be uniformly dissolved in the solvent, and the solid component insoluble in the solvent can be separated from the solution in a stable state. When the melting temperature is lower than the melting point of the wax by more than 20 ° C., the wax component also precipitates, so that it becomes difficult to separate it from the solvent-insoluble component. Further, when the dissolution is carried out at a temperature higher than the melting point by 20 ° C. or higher, a component which is insoluble at a temperature lower than that may be eluted from the solvent-insoluble component, and
It is not preferable because it causes excessive heat history to the melted wax.

In the above step (a), as a method for removing the solvent insoluble matter while maintaining the raw material wax in the range of 20 ° C. above and below the melting point of the wax, a conventionally known solid-liquid separation method is used. You can Specifically, it is possible to use an ordinary filtration operation or sedimentation separation, but in order to perform the operation quickly and sufficiently, a method of forcibly performing solid-liquid separation, for example, vacuum filtration, centrifugation, centrifugal filtration. The method and the like are more preferable.

In the step (a) of the method for purifying the natural crude wax of the present invention, the resinous component which is an unnecessary component contained in the natural crude wax is difficult to dissolve in the solvent of the present invention in the vicinity of the melting point of the wax. By utilizing the property, the wax can be dissolved in the solvent and the resinous component in the wax can be effectively removed by solid-liquid separation while the resinous component is not dissolved.

<Step (b)> In the step (b) of the method for purifying a natural crude wax of the present invention, a solvent is added to the raw wax in an amount of 3 to 30 times the weight of the wax and the mixture is heated to remove the wax content. After the dissolution, the wax solid content which is cooled and deposited is collected by a solid-liquid separation operation. At this time, it is necessary to perform solid-liquid separation so that the solvent content in the wax is 50 to 90%. The amount of the solvent that dissolves the wax is 3 to 30 times, and more preferably 5 to 20 times the weight of the raw wax. If the amount of solvent is less than 3 times the weight of the wax, solid-liquid separation between the wax and the solvent precipitated by cooling becomes practically difficult,
Unable to separate unnecessary components. Further, the more the solvent is used, the more the removal rate of unnecessary components is improved, but at the same time, the elution amount of the wax component is increased and the loss of the wax component is increased. The limit is 30 times the weight. When the wax to be supplied contains a solvent, the amount of the solvent to be added is determined in consideration of the amount of the solvent contained. Therefore, when the amount of the solvent is insufficient, it is added separately, and when it is excessive, the amount of the solvent is adjusted to an appropriate amount by an appropriate method, for example, distillation, and used.

In the step (b), the temperature at which the solid wax content is precipitated by cooling may be around room temperature, but the lower the temperature, the better the wax precipitation. However, depending on the solubility of the solvent in the wax, when the temperature is too low, unnecessary components are precipitated and the selectivity is lowered. Therefore, the temperature is usually -10 ° C or higher, preferably 0 ° C.
The above temperatures are used. Further, if the temperature at the time of cooling is too high, the precipitation of wax solids is not sufficient, and the solvent is likely to be included in the precipitated wax solids,
The cooling temperature should be below 40 ° C.

In the step (b), the raw wax is dissolved in a solvent and then cooled to precipitate the wax solid content, which is solid-liquid separated so that the solvent content in the solid content is 50 to 90%. I do. When the content of the solvent in the solid content of the wax after solid-liquid separation is more than 90%, unnecessary components that destabilize the properties of the wax are not sufficiently removed, and the quality of the product wax deteriorates. Further, the smaller the residual amount of the solvent in the wax is, the more preferable it is. However, considering practical conditions such as an apparatus, the limit is 50%. If it is attempted to remove the solvent more than that, the time and cost for purification are increased, and it is not preferable for the purpose of obtaining uniform quality. In practice, more preferable results can be obtained by performing the solid-liquid separation operation so that the solvent content in the solid wax content is in the range of 60 to 80%. Therefore, in the step (b) of the method for producing a natural crude wax of the present invention, the raw wax is heated in the presence of a solvent in an amount of 3 to 30 times, more preferably 5 to 20 times the weight of the wax. After the wax component is dissolved, the wax solid component deposited by cooling the solid component is solid-liquid separated so that the solvent content in the solid component is in the range of 50 to 90%, preferably 60 to 80%. Do.

In the step (b) of the present invention, the raw wax is dissolved in a solvent and then cooled to precipitate a solid wax, which is solid-liquid so that the solvent content in the solid is 50 to 90%. As a method for separating, for example, suction filtration or the like used in a normal filtration operation can be used, but since it takes a considerable time to reach the above solvent content, solid-liquid separation is more forcibly performed. Is preferred. Specifically, a device such as a centrifugal filtration device or a centrifuge that forcibly separates the solid content from the liquid by using centrifugal force, or a device such as a filter press, a belt press, or a screw press that applies pressure to filter is used. It is desirable to apply.

In the step (b) of the method for purifying the natural crude wax of the present invention, unnecessary components contained in the natural crude wax are glycerides, free unsaturated fatty acids, free sterols, and these fatty acids. By utilizing the property that the sterol ester component or the like in which sterol and sterol are bonded is difficult to crystallize during recrystallization of the wax, solid-liquid separation is performed in a state where these unnecessary components remain dissolved in the solvent, The unnecessary components can be effectively removed, and as a result, a very excellent wax can be obtained.

As the solvent used in steps (a) and (b) of the method for purifying a natural crude wax of the present invention, any solvent can be used as long as it is an organic solvent generally used for solvent purification of waxes. . Particularly, lower alcohols are preferable because they are excellent in extraction efficiency, and more preferably alcohols having 1 to 4 carbon atoms. Examples of these alcohols include methanol, ethanol, 1-
Propanol, 2-propanol, 1-butanol, 2
-Butanol, tert-butanol and the like. In the above steps (a) and (b), different solvents may be used, or the same solvent may be used in both steps.

In the method for purifying a natural crude wax of the present invention, the order of use of the above steps (a) and (b) is appropriately changed depending on the properties of the raw wax and the quality required for the purified product. You can That is, either the method of performing the step (b) after performing the step (a) or the method of performing the step (a) after performing the step (b) can be selected.

As described above, the resinous component contained in the natural crude wax has a specific gravity larger than that of the wax solution, as can be seen from the fact that the wax naturally dissolves when the wax is dissolved in a solvent and left to stand. Therefore, a solvent is added to the natural crude wax to uniformly dissolve the wax component, and the resinous component is suspended without being dissolved, and then the wax component is cooled while gently stirring to precipitate the wax component. As a result, a precipitate of the wax solid content in which the resinous component and the wax content are mixed is formed. This wax solid has a high density because it contains a resinous component, and the difference in density from the solution is larger than when it does not contain a resinous component. Further, the resinous component serves as a nucleus when the wax is crystallized, and crystals with large particles are obtained. By performing solid-liquid separation of the slurry liquid composed of the solution and the solid wax content, it is possible to effectively separate the solution and the solid wax content. That is, by performing the step (b) prior to the step (a), the resinous component present in the natural crude wax in the step (b) is intentionally incorporated into the wax solid content, whereby the solution and the wax solid are solidified. Since the difference in density from that of the solvent increases and solid-liquid separation becomes easier, the amount of solvent used can be reduced. On the other hand, when the step (b) is performed after the step (a), the above effect cannot be obtained. Therefore, in the step (b), the density of the solution is lowered to widen the density difference from the wax solid content, and the separation ability is increased. To increase the amount, a large amount of solvent must be used, which is economically disadvantageous. Therefore, the method of performing the step (b) and then the step (a) is preferable from the viewpoint of separation efficiency.

When the above step (a) is to be performed later,
Since a solvent solution of the purified wax is obtained, the purified wax can be obtained by removing the solvent by a conventional method such as distillation in the step (c). Similarly, when the step (b) is used as a subsequent step, a refined wax having a solvent content of 50 to 90% can be obtained. Therefore, in the same step (c), the solvent should be removed by a conventional method such as distillation. A purified wax is obtained by. It should be noted that other purification methods such as hydrorefining and adsorption treatment can be appropriately employed before and after these steps.

[0020]

The present invention will be described in detail below with reference to examples, but the present invention is not limited thereto.

<Reference production example> Extraction of sugar cane crude wax Extraction of sugar cane crude wax The sugar juice squeezed and squeezed out of the sugar cane in the crude sugar production process is allowed to stand still, and the suspended matter mainly consisting of fibers and fats and oils floating above the juice is filtered. The filter cake obtained by separation was dried in a vacuum constant temperature bath to obtain a dried cake. The dried cake was placed in a container equipped with a stirrer, a reflux condenser and a heating heater, n-heptane was added as an extraction solvent, and the mixture was heated with stirring to extract at the solvent reflux temperature. Immediately after the completion of extraction, filtration was performed to separate and remove the filter cake. The filtrate was allowed to stand, the lower aqueous layer was separated, the heptane layer was distilled, and the solvent was removed to obtain a dark green sugar cane crude wax. The result of DSC (Differential Scanning Calorimetry) of the above sugar cane crude wax was 6
Main peak was seen at 1.0 ℃, 47 ℃ and 75 ℃
A peak was also observed, and it was found that the melting temperature range was broad and wide as a whole. Further, as a result of gas chromatographic analysis, it was found that about 40% of unnecessary components were included as wax.

<Example 1> Step (a): The sugar cane crude wax obtained in the above Reference Production Example was placed in a container equipped with a reflux condenser, a stirrer, and a heater, and 2-propanol was added as a solvent at a weight ratio of 5
The weight was added, and the mixture was heated and stirred for 1 hour while refluxing the solvent to dissolve the wax. At this time, the temperature of the solution was about 4 ° C. higher than the melting point of the raw wax. After confirming that the wax was dissolved in the solvent, set the temperature to 65-7.
While maintaining the temperature at 0 ° C., this was separated by a centrifuge under the condition of 2000 G for 10 minutes. The precipitated solid content and the wax solution were separated by decantation, the solvent was removed by distillation to remove the solvent-insoluble solid content, and a purified sugar cane wax (A) was obtained. Step (b): The refined sugar cane wax (A) from which the solvent-insoluble solid content obtained in the above step (a) has been removed is put in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol is used as a solvent. Is added 15 times by weight to the weight of the wax, and the mixture is heated and stirred for 1 hour while refluxing the solvent,
The wax dissolved. After confirming that the wax was dissolved in the solvent, the mixture was cooled with slow stirring to lower the temperature to 5 ° C., and further left at room temperature for 12 hours with slow stirring.
The slurry-like liquid in which the wax was deposited was filtered under the condition of 1500 G using a centrifugal filter to solid-liquid separate the wax solid content and the solvent. At this time, the residual solvent amount in the solid wax content was 68%. Step (C): The solvent was removed from the obtained wax solid content by distillation to obtain a purified sugar cane wax (B). As a result of DSC of the purified sugar cane wax (B), a single sharp peak was observed at 80.5 ° C., and it was found that the wax was a very meltable sharp wax. As a result of gas chromatographic analysis, it was found that the content of unnecessary components as wax was 5% or less.

<Example 2> Step (b): The sugar cane raw wax obtained in the Reference Production Example was put in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol was used as a solvent based on the weight of the wax. 10 times by weight and heat to reflux the solvent 1
Stir for hours to dissolve the wax. After confirming that the wax was dissolved in the solvent, cool the mixture with slow stirring to lower the temperature to 7 ° C, and further with gentle stirring at room temperature,
Left for hours. The slurry-like liquid in which the wax was deposited was subjected to solid-liquid separation for 10 minutes at 1500 G using a centrifugal filter. The residual amount of the solvent in the wax solid content was 71%. The solvent was removed from the obtained wax solids by distillation to obtain a purified sugar cane wax (C). Step (a): The purified sugar cane wax (C) obtained in the above step (b) is placed in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol is added as a solvent in an amount of 5 times by weight of the wax and added. The wax was dissolved by stirring for 1 hour while warming and refluxing the solvent. At this time, the temperature in the solution was about 3 ° C. higher than the melting point of the raw wax (C). After confirming that the wax was dissolved in the solvent, it was separated by a centrifuge at 2000 G for 10 minutes while maintaining the temperature at 65 to 70 ° C. The precipitated solid content and the wax solution were separated by decantation. Step (c): The solvent in the wax solution was removed by distillation to obtain a purified sugar cane wax (D). As a result of DSC of the purified sugar cane wax (D), a single sharp peak was observed at 81.0 ° C., and it was found that the wax was a very meltable sharp wax. As a result of gas chromatographic analysis, it was found that the content of unnecessary components in the wax was 4% or less.

Comparative Example 1 The sugar cane crude wax obtained in the above Reference Production Example was placed in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol was added as a solvent in an amount of 5 times by weight based on the weight of the wax. The wax was dissolved by stirring for 1 hour while heating and refluxing the solvent. After confirming that the wax was dissolved in the solvent, the wax was cooled with slow stirring to lower the temperature to 5 ° C., and further left at room temperature for 18 hours with slow stirring. The slurry-like liquid in which the wax was deposited was subjected to solid-liquid separation by a centrifugal filter at 1500 G for 5 minutes. At this time, the residual solvent amount in the solid wax content was 83%. The solvent was removed from the obtained wax solids by distillation to obtain a purified sugar cane wax (E). DSC result of refined sugar cane wax (E) shows 80.1
In addition to the main peak at 7 ° C, a peak also appeared at 74.7 ° C, which is relatively broad as a whole, and has a wider melting temperature range than the refined sugar cane waxes (B) and (D). I knew that. Further, when the hardness of this refined sugar cane wax (E) was compared with that of the above refined sugar cane waxes (B) and (D), it was found to be brittle and easily broken.

<Comparative Example 2> The sugar cane crude wax obtained in the above Reference Production Example was put in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol was added as a solvent in an amount of 5 times by weight of the wax and heated. And then reflux the solvent 1
Stir for hours to dissolve the wax. At this time, the temperature in the solution was about 4 ° C. higher than the melting point of the wax. After confirming that the wax has dissolved in the solvent, increase the temperature to 6
Using a centrifuge, keep this at 5 to 70 ° C.
Separation was performed for 10 minutes under the condition of 00G. The precipitated solid content and the wax solution were separated by decantation, and the solvent was removed by distillation to obtain a purified sugar cane wax (F).
DSC result of refined sugar cane wax (F) shows 7
The main peak was seen at 6.2 ° C, as well as 64.7 ° C and 53.
It was found that a peak appeared at 4 ° C., which was broad as a whole, and had a wide melting temperature range. In addition, as a result of gas chromatographic analysis, it was found that about 23% of unnecessary components were included as wax. Further, this refined sugar cane wax (F) was quite soft and was not suitable as a hard wax.

<Comparative Example 3> Step (b): The sugar cane crude wax obtained in the Reference Production Example was placed in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol was used as a solvent based on the weight of the wax. 5 times by weight, and the mixture was heated and stirred for 1 hour while refluxing the solvent to dissolve the wax. After confirming that the wax was dissolved in the solvent, the wax was cooled with slow stirring to lower the temperature to 5 ° C., and further left at room temperature for 18 hours with slow stirring. The slurry-like liquid in which wax was deposited was filtered by a suction filter for 1 hour to perform solid-liquid separation. At this time, the residual solvent amount in the solid wax content was 93%. The solvent was removed from the obtained wax solids by distillation to obtain a purified sugar cane wax (G). Step (a) -step (c): The purified sugar cane wax (G) obtained in the above step (b) is put in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol is used as a solvent for the wax 2. The weight was added, and the mixture was heated and stirred for 1 hour while refluxing the solvent to dissolve the wax. At this time, the temperature in the solution was about 3 ° C. higher than the melting point of the raw wax (G). After confirming that the wax was dissolved in the solvent, the wax was separated by a centrifuge at 2000 G for 10 minutes while maintaining the temperature at 60 to 65 ° C. The precipitated solid content and the wax solution were separated by decantation, and the solvent was removed by distillation to obtain a purified sugar cane wax (H). DSC of refined sugar cane wax (H)
The result showed that the main peak was found at 64.4 ° C and 4
It was found that peaks also appeared at 9.9 ° C and 76.4 ° C, which were broad as a whole, and had a wide melting temperature range. As a result of gas chromatographic analysis, it was found that about 17% of unnecessary components as wax were contained.
It was found that the refined sugar cane wax (H) was much softer and easier to collapse than the refined sugar cane waxes (B) and (D), and was inferior as a hard wax.

<Example 3> Step (b): The sugar cane crude wax obtained in the Reference Production Example was placed in a container equipped with a reflux condenser, a stirrer and a heater, and ethanol was used as a solvent in an amount of 10 based on the weight of the wax.
The weight was added, and the mixture was heated and stirred for 1 hour while refluxing the solvent to dissolve the wax. After confirming that the wax was dissolved in the solvent, cool the mixture with slow stirring to bring the temperature to 7
The temperature was lowered to 0 ° C., and the mixture was allowed to stand at room temperature for 24 hours with slow stirring. The slurry-like liquid in which the wax was deposited was subjected to solid-liquid separation using a centrifugal filter under the condition of 1500G. At this time, the residual solvent amount in the solid wax content was 75%. The solvent was removed from the obtained solid wax by distillation to obtain a purified sugar cane wax (J). Step (a) -step (c): The purified sugar cane wax (J) obtained in the above step (b) is put in a container equipped with a reflux condenser, a stirrer and a heater, and 2-propanol is used as a solvent in the wax 5 The weight was added, and the mixture was heated and stirred for 1 hour while refluxing the solvent to dissolve the wax. At this time, the temperature in the solution was about 3 ° C. higher than the melting point of the wax. After confirming that the wax has dissolved in the solvent,
While maintaining the temperature at 70 to 75 ° C., this was separated by a centrifuge under the condition of 2000 G for 10 minutes. The precipitated solid content and the wax solution are separated by decantation, and the solvent is removed by distillation to obtain a refined sugar cane wax (K).
Got As a result of DSC of the purified sugar cane wax (K), a single sharp peak was observed at 78.1 ° C., and it was found that the wax was a very meltable sharp wax. Also,
As a result of gas chromatographic analysis, it was found that the content of unnecessary components in the wax was 5% or less.

Example 4 The same procedure as in Example 3 was carried out except that ethanol was used in an amount of 15 times the weight of the sugar cane crude wax in the step (b), and the refined sugar cane wax (L) was obtained in the step (b). The refined sugar cane wax (M) was obtained in the step (a). As a result of DSC of the purified sugar cane wax (M), a single sharp peak was observed at 79.8 ° C., and it was found that the wax was a very meltable sharp wax. As a result of gas chromatographic analysis, it was found that the content of unnecessary components as wax was 5% or less.

<Example 5> Step (a): The crude bead wax is put in a container equipped with a reflux condenser, a stirrer and a heater, and the solvent is used as 2-
Propanol was added 5 times the weight of the wax, and the mixture was heated and stirred for 1 hour while refluxing the solvent to dissolve the wax. At this time, the temperature of the solution is 16 higher than the melting point of the raw wax.
The temperature was about ℃ higher. After confirming that the wax was dissolved in the solvent, the wax was separated by a centrifuge at 2000 G for 10 minutes while maintaining the temperature at 60 to 65 ° C. Purified bead wax (O) obtained by separating the precipitated solid content and the wax solution by decantation and removing the solvent by distillation to remove the solid content insoluble in the solvent.
Got Step (b) -Step (c): Put the purified bead wax (O) from which the solvent-insoluble solid content obtained in the above step (a) has been removed into a container equipped with a reflux condenser, a stirrer and a heater. 2-Propanol as a solvent was added in an amount of 15 times the weight of the wax, and the mixture was heated and stirred for 1 hour while the solvent was refluxed to dissolve the wax. After confirming that the wax was dissolved in the solvent, the mixture was cooled with slow stirring to lower the temperature to 5 ° C., and further left at room temperature for 12 hours with slow stirring. The slurry-like liquid in which the wax was deposited was filtered under the conditions of 1500 G using a centrifugal filter to perform solid-liquid separation of the wax solid content and the solvent. At this time, the residual solvent amount in the solid wax content was 73%. The solvent was removed from the obtained wax solids by distillation to obtain a purified bead wax (P). As a result of DSC of the purified beeswax (P), a sharp main peak was observed at 65.5 ° C.
Although a minute peak was observed at ℃, it was found that the wax as a whole had a sharp melting property. In addition, as a result of gas chromatographic analysis, it was found that the unnecessary component as a wax was 7% or less.

<Example 6> Step (a): Crude rice wax was put in a container equipped with a reflux condenser, a stirrer and a heater and used as a solvent.
Propanol was added 5 times the weight of the wax, and the mixture was heated and stirred for 1 hour while refluxing the solvent to dissolve the wax. At this time, the temperature of the solution is 2 ° C. higher than the melting point of the raw wax.
It was a high temperature. After confirming that the wax was dissolved in the solvent, the wax was separated by a centrifuge at 2000 G for 10 minutes while maintaining the temperature at 65 to 70 ° C. The precipitated solid content and the wax solution were separated by decantation, and the solvent was removed by distillation to obtain a purified rice wax (Q) from which the solvent-insoluble solid content was removed. Step (b) -step (c): Put the purified rice wax (Q) from which the solvent-insoluble solid content obtained in the above step (a) has been removed into a container equipped with a reflux condenser, a stirrer and a heater. 2-Propanol as a solvent was added in an amount of 15 times the weight of the wax, and the mixture was heated and stirred for 1 hour while the solvent was refluxed to dissolve the wax. After confirming that the wax was dissolved in the solvent, the mixture was cooled with slow stirring to lower the temperature to 5 ° C., and further left at room temperature for 12 hours with slow stirring. The slurry-like liquid in which the wax was deposited was filtered under the conditions of 1500 G using a centrifugal filter to perform solid-liquid separation of the wax solid content and the solvent. At this time, the residual solvent amount in the solid wax content was 70%. The solvent was removed from the obtained wax solids by distillation to obtain a purified rice wax (R). As a result of DSC of the purified wax (R), a single sharp peak was observed at 81.3 ° C., and it was found that the wax was a very meltable sharp wax. Also,
As a result of gas chromatographic analysis, it was found that the content of unnecessary components in the wax was 5% or less.

[0031]

EFFECTS OF THE INVENTION By performing a refining operation in which the steps (a) and (b) of the present invention are appropriately combined and then the step (c) is carried out, unnecessary components in the raw wax can be effectively removed, and the performance is improved. A very good wax can be obtained. That is, according to the method of the present invention, it is possible to produce a hard wax having a substantially single melting point, a low content of unnecessary components in gas chromatographic analysis, and a low hardness. Furthermore, in order to impart emulsifying property to the oil component once separated, by adding an appropriate amount again,
There is also an effect that it is possible to design wax products.

Claims (4)

[Claims] 1. A method for purifying a natural crude wax, which comprises any of the following steps (a) and (b) in any order, and the following step (c) to be performed thereafter, step (a): weight ratio of wax component to solvent Is 1: 3 to 2
The wax component is dissolved by heating the mixture of 0 to a temperature range of 20 ° C. above and below the melting point of the wax, and the solvent-insoluble component is separated and removed from the solution by a solid-liquid separation operation while maintaining the temperature range. Step, Step (b): Weight ratio of wax component to solvent is 1: 3 to 3
The wax content is dissolved by heating the mixture of 0 to a temperature range of 20 ° C. above and below the melting point of the wax, and then the solid content of the wax is precipitated by cooling, whereby the solvent content in the solid content of the wax is reduced. A step of separating and recovering the wax solid content by a solid-liquid separation operation so as to be 50 to 90%, and a step (c): Among the steps (a) and (b),
A step of obtaining a purified wax by removing the solvent from the wax solution or the solid wax content obtained from the subsequent step. 2. The method for purifying a natural crude wax according to claim 1, wherein the step (b) is carried out first, and then the step (a) is carried out. 3. Of the steps (a) and (b),
The method for refining a natural crude wax according to claim 1 or 2, wherein the wax component used in the previous step is a crude wax extracted from sugar cane. 4. The method for purifying a natural crude wax according to claim 1, wherein the solvent is an alcohol having 1 to 4 carbon atoms.