JPH0711284A - Method for extracting sugar cane wax composition - Google Patents

Abstract

PURPOSE:To extract the high-purity subject compound in high yield and excellent economic efficiency by adding ethanol to the residue in squeezing process of sugar cane and heating the residue under pressure, filtering the mixture and depositing crystals material from the filtrate. CONSTITUTION:Ethanol (preferably water-containing alcohol) is added to the residue obtained in squeezing process in producing sugar from cane wax so that alcohol concentration becomes >=50wt.% ZM, (preferably 70-90wt.%) and the mixture is heated to the boiling point or above (preferably 100-150 deg.C) of ethanol under pressure (preferably 2-5kg/cm<2>) and solid content is filtered in heating and crystals are deposited from the filtrate to extract the objective composition. Furthermore, the residue is preferably a filter cake obtained in cleaning process of sugar.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a method for extracting a sugarcane wax composition.

[0002]

BACKGROUND OF THE INVENTION Sugarcane wax is a white waxy substance which is mainly present on the surface of sugarcane bark and is considered to play a role of protecting the bark. In recent years, higher alcohols such as octacosanol contained in the wax have been utilized in health foods or pharmaceuticals as physiologically active substances, and have attracted attention in various fields including the production of lubricants for OA equipment.

In order to produce such sugarcane wax, the following methods have been conventionally used. That is, the sugarcane residue obtained by squeezing the harvested sugarcane by pressing the harvested sugarcane (so-called bagasse or filter cake, most of which is used as livestock feed or fuel).
Is used as a raw material, and after being sufficiently dried, the boiling point is 95 to
Add about 10 times the volume of petroleum naphtha at 105 ° C and boil,
It is filtered to separate a solid (residue) and a liquid (extract). Then, naphtha is distilled and recovered from this extract to obtain a solid residue.

In addition to wax, this residue contains oil,
Resin content, since it contains tar content such as pitch, ethanol, isopropanol, acetone, after adding an organic solvent such as butyl alcohol, after heating to dissolve,
The black tar content is filtered off by filtration at about 75 ° C. The filtrate thus obtained is cooled to around room temperature to precipitate a wax component, which is then filtered to collect the wax component. Most of the organic solvent used is recovered by distilling the filtrate.

The sugar cane wax produced by such a method has the following problems and is difficult to be industrialized on a large scale until now. That is, in the conventional method, (1) naphtha is inexpensive as an extraction solvent, but there is a concern in terms of safety. (2) The naphtha extract contains a large amount of impurities other than the target wax component, and a hydrophilic organic solvent such as a lower alcohol is required to purify the impurities. However, the combined use of such a solvent and naphtha is a production facility. This not only complicates the equipment and equipment but also increases the manufacturing cost. Therefore, it has been desired to develop a method of performing extraction and purification with a single solvent, which is preferably highly safe, but an effective means has not been found.

It is possible to use, for example, a lower alcohol as such an extraction solvent, but in order to improve the extraction efficiency of a lipid component such as wax, a lower alcohol is used as a solvent having an extremely low water content. Must. However, in the case of sugarcane residue used as a raw material, for example, that generated in the sugar cleaning process, it is usually 70 to 8
Since it contains about 0% of water, the actual extraction process must be carried out in a water-containing system. In such a system, impurities (oil, resin, pitch, etc.) other than wax as well as the wax itself The extraction rate was also significantly reduced, and as a result, it was difficult to increase the extraction efficiency such as the purity and yield of the target product. Further, in order to remove the water content of the raw material and the water content of the recovered solvent, a large amount of equipment and cost are required.

[0007]

SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a method for efficiently extracting a high-quality sugarcane wax composition using sugarcane residue as a raw material and a highly safe single solvent. Especially.

[0008]

In order to solve the above problems, the inventors of the present invention have earnestly studied, and as a result, the present inventors have conducted an extraction treatment at high temperature and pressure using hydrous alcohol, and then cooled the extracted liquid to remove the wax content. It has been found that a high quality sugarcane wax composition can be obtained by precipitation. The present invention has been completed based on such findings. That is, the gist of the present invention is to add ethanol so that the alcohol concentration is 50% by weight or more to the residue obtained in the pressing step when sugar is produced from sugar cane, and after heating under pressure to the boiling point of ethanol or higher. A method for extracting a sugarcane wax composition is characterized in that a solid content is filtered off when heated and a crystalline substance is precipitated from the filtrate.

The raw material used in the present invention is a raw material used in the step of producing sugar from sugar cane by a known method.
It is the residual obtained when the sugar cane is pressed and in the subsequent pressing step, and examples of such a residue include bacas during the pressing of sugar cane and filter cake generated in the sugar cleaning step. These residues are usually obtained as a water-containing material, and in the present invention, the water-containing material can be applied as it is, but it is preferable to dry it in view of workability and manufacturing cost.

Ethanol is used as the extraction solvent, and is adjusted so that the alcohol concentration in the system when added to the raw material is 50% by weight or more. If it is less than 50% by weight, the extraction rate of the target wax component will decrease. Therefore, in the present invention, ethanol having various water contents depending on the water content of the raw material can be used, and high-purity non-aqueous ethanol is not necessarily used. From the viewpoint of recovery and reuse of the extraction solvent, it is preferable to use hydrous ethanol, and the ethanol concentration is 55% by weight or more, preferably 70 to 90% by weight. If it is less than 55% by weight, it becomes substantially difficult to set the alcohol concentration in the system to 50% by weight or more, and the desired wax component cannot be efficiently extracted.

Next, in the present invention, the mixture of the raw material and ethanol is heated to a boiling point of ethanol or higher under pressure. The degree of pressurization is 2 kg / cm ² or more, preferably 3 to 5
It is kg / cm ² , and if it is less than 2 kg / cm ² , the extraction rate of the target substance is low, and conversely, if the pressure exceeds 5 kg / cm ² , further extraction efficiency cannot be expected. The heating is performed at the boiling point of ethanol or higher, preferably 100 to 150 ° C. Heating below the boiling point of ethanol results in low extraction rate and purity of the extract.
Even if the temperature exceeds 50 ° C, there is no great difference from the effect of the present invention. In such a pressurized and heated state, stirring is preferably carried out to enhance the contact between the raw material and ethanol, and the extraction treatment is carried out for 1 to 4 hours.

The mixture thus obtained is filtered while heating, preferably at 75 to 85 ° C., by a known method, to separate into a solid content and a filtrate. At this time, when the temperature is lower than 75 ° C., the target substance is precipitated and removed by filtration treatment, resulting in a decrease in yield. Then, cool the filtrate to room temperature (25 ° C) or lower,
At this time, a yellow to white crystalline substance precipitates, and the target sugarcane wax composition can be obtained by filtering this. If the filtrate is recovered and subjected to simple distillation, it can be purified as hydrous ethanol having an ethanol concentration of about 90%, and can be reused as an extraction solvent.

[0013]

EXAMPLES In the following examples and comparative examples,% is based on weight. Example 1 A dried product of a filter cake containing 4% of a wax component (water content of 20 obtained in the step of cleaning sugar cane juice juice).
%) 100 g into a pressure vessel equipped with a stirrer, add 800 ml of 90% ethanol, pressurize to 3 kg / cm ² , and press 120
The mixture was stirred at 0 ° C for 2 hours. Then, filtration was performed at 80 ° C. to separate a solid content and a filtrate. Cool the filtrate to 25 ° C., 5
After allowing it to stand for a period of time to precipitate crystals, the crystals were filtered off. The crystal yield was 3.9 g, and the melting point was 78 to 82 ° C. When this crystal product was further decolorized with 35% hydrogen peroxide, it turned pale yellow.

Example 2 The same apparatus and raw materials as in Example 1 were used. That is, to 100 g of dried filter cake (water content 10%),
1500 ml of 70% ethanol was added, the pressure was increased to 4 kg / cm ² , and the mixture was stirred at 140 ° C. for 2 hours. Then, filtration was performed at 80 ° C. to separate a solid content and a filtrate. The filtrate was allowed to stand at 25 ° C. for 6 hours, and the precipitated crystal substance was filtered off. The crystal yield was 3.9 g, and the melting point was 78 to 82 ° C.

Comparative Example 1 Using the same equipment and raw materials as in Example 1, extraction was carried out without pressurization. That is, 800 ml of 90% ethanol was added to 100 g of the dried filter cake (water content 20%), and the mixture was stirred at 75 ° C. for 2 hours under normal pressure. Then, filtration was performed at 80 ° C. to separate a solid content and a filtrate. 25 filtrate
The mixture was cooled to 0 ° C. and allowed to stand for 5 hours, and the precipitated crystal was filtered off. The yield of crystals is as low as 1 g and the melting point is 70-
It was 75 ° C.

Comparative Example 2 Using the same apparatus and raw materials as in Example 1, extraction was performed without heating. That is, dry filter cake (water content 20
%) 800 g, 90% ethanol 800 ml was added, the pressure was increased to 4 kg / cm ² with nitrogen, and the mixture was stirred at 25 ° C. for 2 hours. Then, it filtered at 25 degreeC and isolate | separated into solid content and a filtrate. The filtrate was allowed to stand at 25 ° C. for 5 hours, but no crystalline substance was deposited.

Example 3 In the method described in Example 1, the raw material was replaced with a semi-dried product (moisture content of 40%) of the same filter cake, which was once used for extraction treatment and subjected to simple distillation treatment to recover 2000 ml of 90% ethanol. Was used under the same conditions as above. As a result, the yield of the crystalline product was 3.8 g, and the melting point was 78 to 82 ° C.

Example 4 In the method described in Example 1, the raw material was a squeeze residue of sugar cane (water content 5%, wax content: 0.2%).
The treatment was carried out under the same conditions except that 2000 ml of 90% ethanol was used. The yield of the obtained crystal product is 0.1.
8 g, melting point 78-82 ° C.

[0019]

EFFECTS OF THE INVENTION According to the present invention, inexpensive residue derived from sugar cane is used as a raw material, and only highly safe ethanol used in foods is used. It is possible to extract a high-purity sugarcane wax composition with high purity. Moreover, this method is excellent in economic efficiency because the extraction solvent can be easily distilled, recovered and reused.

Claims (5)

[Claims] 1. To the residue obtained in the pressing step when sugar is produced from sugar cane, ethanol is added so that the alcohol concentration becomes 50% by weight or more, and the mixture is heated to a boiling point of ethanol or higher under pressure and then heated. A method for extracting a sugarcane wax composition, characterized in that a solid matter is sometimes filtered off to precipitate a crystalline substance from the filtrate. 2. The method according to claim 1, wherein the residue is a filter cake generated in the sugar cleaning step. 3. The method according to claim 1, wherein the ethanol is a hydrous alcohol and the ethanol concentration is 70 to 90% by weight. 4. The method according to claim 1, wherein the pressurization is performed at 2 to 5 kg / cm ² . 5. The heating is performed at 100 to 150 ° C.
The method described.