KR100239179B1 - Beeswax manufacturing method - Google Patents

Abstract

After honey is separated from the honeycomb of Apis cerana, the honeycomb is heated and dissolved in hot water to leave a solid beeswax solidified on top. The method for producing beeswax is obtained by adding and stirring a phosphate solution to a liquid beeswax, which is heated and dissolved, and then washed with water, adsorbed with a mixture of activated carbon and activated clay, decolorized, and exposed to steam to deodorize. The process is stable and simple, and the device is simple and offers excellent purification, which is of great industrial utility. In particular, when honey producers produce dense bees, they can use small subdivision facilities, a facility that separates honey from honeycombs.

Description

Beeswax manufacturing method

[Industrial use]

The present invention relates to a method for manufacturing beeswax, and more particularly, honeycomb for use in various industries such as raw materials, adhesives, waterproofing agents, lubricants, dental materials, cosmetics, pharmaceuticals, food, etc. The present invention relates to a method for preparing beeswax by separating and collecting beeswax from to remove impurities and phosphoric acid treatment, decolorization and deodorization.

[Prior art]

Beeswax is an expensive raw material of the highest quality among animal and animal waxes and artificial waxes used for similar purposes as a collection of waxes obtained from honeycomb.

As an example of the method of manufacturing beeswax, Japanese Patent Publication No. 57-25596 discloses a method of decolorizing and deodorizing beeswax. However, this method uses ozone (O ₃ ), which requires complex facilities and confined spaces, and poses a risk of human exposure to ozone during the process. It is already known that exposure to ozone causes dizziness and even death. In addition, since high ozone or lack of oxygen is difficult to generate ozone, there are many difficulties in decolorizing beeswax at a temperature used in the method, 60 ° C to 120 ° C. Due to various problems as described above, the method is very difficult to apply in an actual industrial field.

Beeswax components are different depending on the type of bee, the type of honey, bee collecting, region and time, the manufacturing method may also vary, it is preferable to develop and apply the optimal manufacturing method according to the components of beeswax.

In general, bees can be classified into bees from Apis mellifera and bees from Apis cerana. The former has high acid value and the latter has low acid value. Currently, beeswax used for industrial purposes is mostly beeswax derived from Apis mellifera, because the beeswax beeswax produced by Apis mellifera, a Western bee, is mostly supplied in Europe, the United States, and Africa.

In Japan, Cerarica Noda is researching low-acid beeswax and identifying other characteristics of high-value beeswax and using its advantages to develop unique uses. We are researching bleaching methods.

U.S. Patent No. 2,406,336 discloses a method of modifying the physical properties of the wax, such as melting point, acid value, saponification value, and the like, for use as a brightening agent.

An object of the present invention is to provide a method for producing beeswax, which is simple in facilities and processes, has no risk to the human body, is easy to apply on an industrial scale, is advantageous for mass production, and exhibits excellent refining ability, in particular, Apis cerana. This is to provide a method for preparing beeswax which is very suitable for the production of beeswax derived.

1 is a diagram schematically showing an apparatus that can be used in the bleaching process of the method of manufacturing beeswax according to an embodiment of the present invention.

Figure 2 is a diagram schematically showing an apparatus that can be used in the deodorization process of the method of manufacturing beeswax according to an embodiment of the present invention.

<Explanation of symbols for main parts of drawing>

1, 15: vacuum pump 2: beeswax inlet

3: glass filter 5: filter paper

7: magnetic bar 19: liquid nitrogen trap

23 condenser 31 steam injector

33: deodorization tank

In order to achieve the above object of the present invention, the present invention provides a process for adsorbing crude beeswax into a mixture consisting of activated carbon and activated clay to decolorize and deodorizing the decolored beeswax by exposing it to steam. It provides a method for producing beeswax comprising. As a pretreatment step of the decolorizing step, it is preferable to further include a step of heating and liquefying the dense bees, followed by adding and stirring the phosphoric acid solution and then washing with water.

As another aspect of the present invention, the present invention provides a process for separating honey from a honeycomb of Apis cerana, a step of heating water by adding water to the remaining honeycomb after the honey is separated, and a process of cooling a mixture of liquids obtained by the heating process. And a step of separating the solid beeswax obtained by the cooling step, a step of heating and liquefying the beeswax, a step of adding and stirring a phosphate solution to the liquefied beeswax, and a beeswax stirred by adding the phosphate solution. It provides a method for producing beeswax comprising the step of washing with water and the step of adsorbing the washed beeswax with a mixture of activated carbon and activated clay and decolorizing the exposed beeswax by steam.

The process of washing with water after adding and stirring the phosphoric acid solution used in the method of preparing beeswax of the present invention increases the decolorization efficiency and serves to remove gum substances such as phospholipids remaining in the dense beeswax. It is preferable to use distilled water especially at the time of washing with water, and washing with water until it becomes pH 5-pH6 is preferable. In the phosphoric acid treatment step, the concentration of the phosphoric acid solution is preferably 35 to 45% phosphoric acid solution, and more preferably 40% phosphoric acid solution. The phosphoric acid solution is preferably added at 0.05 to 0.5% by weight of the crude beeswax. If the phosphoric acid solution is added at less than 0.05% by weight, it is difficult to remove the sample material contained in the dense bees, and the decolorizing power is decreased during the decolorizing process. There is a problem in that the yield is lowered. In the step of adding and stirring the phosphoric acid solution, the stirring time is preferably performed for 25 to 35 minutes.

In the methods for producing beeswax of the present invention, the pressure of the decolorizing process is preferably vacuum. The effect of oxygen in the decolorization process increases free fatty acids and raises the melting point, which is prominent in oxygen and high temperature environments and can have a significant effect on color. It is preferable that the adsorption time of the said decolorization process is 30 minutes-50 minutes. The adsorption time of beeswax in the decolorizing process is an important factor in determining the economy and yield. As the adsorption time increases, the decolorizing effect is excellent, but in view of economical efficiency and overall process time, the adsorption time is preferably 30 minutes to 50 minutes, and more preferably 30 minutes to 40 minutes. It is preferable that the temperature of the said decolorization process is 70 degreeC-200 degreeC. Since the main component of beeswax is ester-based and the color of the pigment is a carotene-based pigment, temperature is a very important factor in the decolorizing process. If the decolorizing process is performed at a temperature of less than 70 ° C., the wax may not be sufficiently melted, and the reaction may be difficult. In severe temperature conditions of more than 200 ° C., the recombination reaction of the dye and the diversity of the dye may occur. The amount of the mixture consisting of activated carbon and activated clay used in the decolorizing process is preferably 2 to 10% by weight of beeswax added to the decolorizing process. In the present invention, the mixture consisting of activated carbon and activated clay used as the adsorbent increases the decolorizing effect as the amount is used, but the oil retention of beeswax remaining in the adsorbent increases, so that the yield is lowered, and before entering into the deodorizing process. There is a disadvantage in that the filtration time for removing the adsorbent used in the decolorizing process becomes long. The mixed weight ratio of activated carbon and activated clay of the mixture consisting of activated carbon and activated clay used in the decolorizing process is preferably 45:55 to 55:45. The adsorbent used in the present invention is a mixture consisting of activated carbon and activated clay, and in general, activated carbon having a large specific surface area is known to have better decolorizing ability than activated clay. However, since activated carbon has a higher price than activated clay and a large amount of oil retention of beeswax, proper mixing ratio of activated carbon and activated clay is a very important factor. When activated carbon is used alone than when mixed with activated clay, the color of beeswax is increased, and the activated carbon particles are very fine, which makes it difficult to completely separate activated carbon, and activated carbon remains in the wax.

In the manufacturing method of the beeswax according to the present invention, the temperature of the deodorization process is preferably 80 ℃ to 300 ℃. If the temperature is less than 80 ℃ deodorization by steam is not made properly, at a temperature higher than 300 ℃ may cause the complex compound in the wax to decompose and recombine. The pressure condition of the deodorization process is preferably from vacuum to 0.3 atm. The lower the pressure during deodorization, that is, the higher the degree of vacuum, the better the deodorizing effect. This is thought to be because the chemical structure of beeswax becomes unstable in the presence of oxygen. The time required for the deodorization process is preferably 1.5 to 2 hours. The longer the exposure time of the wax to the vapor during deodorization, the better the effect. However, appropriate adjustments are necessary to avoid excessive delays in the overall process time. The amount of steam used in the deodorization process is preferably 2 to 10% by volume / weight (v / w)% of the beeswax added to the deodorization process.

The beeswax used in the method for producing beeswax according to the present invention is preferably beeswax derived from Apis cerana, but can also be applied to beeswax derived from Apis mellifera.

The inventors of the present invention investigated the components of beeswax derived from Apis cerana before inventing the method for preparing beeswax. As a result, the acid value was 4-5, the peroxide value was 1-8, the saponification value was 60-100, the iodine value was 10 -15 and ester value were 40-60 and melting | fusing point was 64-66 degreeC. The fatty acid was methylated and separated by gas chromatography and mass spectrometry. The components identified by Covet's index were 15 saturated fatty acids having 14 to 28 carbon atoms and 2 unsaturated fatty acids having 18 carbon atoms. The identified hydrocarbons were identified from 23 to 31 carbon atoms.

The following presents a preferred embodiment to aid the understanding of the present invention. However, the following examples are provided only to more easily understand the present invention, and the present invention is not limited to the following examples.

EXAMPLE

Apis cerana honeycomb was used as raw material. As primary rendering, 2 kg of raw material was placed in a flask at a weight ratio of water and 1: 1, heated to 80 to 90 ° C., filtered using gauze, and cooled until the wax was hardened. The beeswax in the solidified form was separated, placed in a flask, added with the same amount of water, heated at 80 to 90 ° C., subjected to secondary rendering, filtered using gauze, and cooled until the wax was hardened. Some of the crude beeswax thus obtained are heated and liquefied as a pretreatment step of the decolorizing process, and then 40% phosphoric acid solution is added to 0.2% by weight of the crude beeswax, stirred and washed with a large amount of distilled water to adjust the pH. It was prepared, and the remaining beeswax was prepared in the form of beeswax without undergoing the phosphoric acid solution treatment process.

Next, a mixture of activated carbon and activated clay was prepared as an adsorbent used in the decolorizing process. The specific surface area and pore size of the activated carbon and activated clay to be used in this example were investigated in advance, and the results are shown in Table 1.

In this example, as shown in Table 1 above, the active clay 1 having excellent specific surface area characteristics was selected and used.

The activated carbon and activated clay 1 were mixed at various ratios from 0: 100 to 100: 0 to prepare an adsorbent. Beeswax, which was previously treated by phosphorication and beeswax, was added to the apparatus of FIG. 1 together with an adsorbent. At this time, the amount of the adsorbent was varied in 1 to 9% by weight of the beeswax added. 1 is a device generally used in a laboratory as a device capable of simultaneously liquefying beeswax, stirring with an adsorbent, and filtering, and those skilled in the art will be able to easily apply the device on an industrial scale. . In order to prevent the reaction with oxygen, the entire system was maintained at 10 ^-4 torr using a vacuum pump (1) and helium gas to prevent discoloration due to contact with the adsorbent and contact with oxygen during filtration. Heating was carried out variously at 60 to 200 ℃ using a thermostat, and the reaction time with the adsorbent was also subjected to a decolorization process by applying a variety of temperatures to 10 to 60 minutes and filtered. The filtration method was first passed through the filter paper (Whatman No. 2) (5), and then passed through the glass filter (3), and filtered by using a pressure difference filled with helium gas to avoid contact with oxygen. In addition, in the apparatus of FIG. 1, the decolorization process was performed under normal pressure without operating the system for maintaining the vacuum. That is, the decolorization process was performed by changing only the pressure conditions and the other conditions in the same manner. After the decolorization process, it was decolorized by spectrophotometric method proposed by American Oil Chemists' Society (spectrophotometer: Model No. 6100, Jenway, USA) and Lovibond system (Lovibond model E tintometer: Model No. AF900, UK, Tintometer). The degree of was measured. Spectroscopic color in the spectroscopy was calculated by the following equation (1).

In the above formula, A represents absorbance.

In particular, since the wax is solid at room temperature, hot water is circulated in the spectrophotometer cell block to maintain a constant temperature (80 ° C.) so that the wax does not solidify.

The beeswax was decolorized and filtered and then fed to the deodorizer shown in FIG. 2. 2 is a device generally used in a laboratory, and those skilled in the art will be able to easily apply the device on an industrial scale. As shown in FIG. 2, the deodorization tank 33 was made of pyrex, 50 mm in diameter, and 120 mm in length, and the steam distributor 31 used a glass filter disk having a diameter of 20 mm. It was. All steam inlet lines were wrapped with a linear heating coil to maintain a temperature of 110 ° C. to prevent condensation of the steam. 1 degreeC water was made to flow into the condenser 23 using the thermostat, and the condensation performance of water vapor was improved. A liquid nitrogen trap 19 was set up for the collection of the fragrance components and two traps were installed to prevent clogging of the trap. A three-way stopcock was installed in front of the trap to regulate the performance of the pump 15 by flowing nitrogen gas in the middle of the line and to change the system pressure. In the apparatus of FIG. 2, the deodorization process was performed by variously adjusting the conditions to a temperature of 100 to 250 ° C., a pressure of 0.3 to 1 atmosphere, a time of 0.5 to 2 hours, and a vapor amount of 1 to 7%.

The experimental results of the above examples are shown in Tables 2 to 9 below.

Table 2 below shows 50 wt% of activated carbon and activated clay in the adsorbent used in the decolorization process, and added beeswax prepared by washing with phosphoric acid solution. , The adsorption time, that is, the stirring time is 60 minutes and the decolorization results are shown after the decolorization process with only the pressure conditions.

As shown in Table 2 above, it can be seen that the decolorizing process in a vacuum state than in normal pressure shows an excellent decolorizing effect.

Table 3 below shows the wax prepared by washing with phosphoric acid solution after washing with water, the mixture weight ratio of activated carbon and activated clay in the adsorbent used in the decolorization process is 50:50, the amount of adsorbent is 5% by weight of the added beeswax, and the adsorption temperature is 80 ° C. After desorption process under different adsorption time, that is, only stirring time under vacuum, the results are shown.

As shown in Table 3 above, it can be seen that the optimum adsorption time, that is, the stirring time of the adsorbent and beeswax is in the range between 30 minutes and 50 minutes.

Table 4 shows the wax prepared by washing with phosphoric acid solution after washing with water, the mixture weight ratio of activated carbon and activated clay in the adsorbent used in the decolorizing process of the above embodiment is 50:50, the amount of adsorbent is 5% by weight of the input beeswax, adsorption time 60 The results are shown after the decolorization process with different adsorption temperatures only under minutes and vacuum.

As shown in Table 4 above, it can be seen that the difference in chromaticity does not appear significantly between the melting point of the wax and 100 ° C.

Table 5 below shows the beeswax prepared by washing with a phosphoric acid solution and washed with water, and the mixed weight ratio of activated carbon and activated clay in the adsorbent used in the decolorizing process of the embodiment is 50:50, adsorption temperature is 80 ℃, adsorption time is 60 minutes, vacuum The results are shown after the decolorization process was carried out by varying only the dose of the adsorbent.

As shown in Table 5, the amount of adsorbent added showed a sharp decrease in chromaticity in the region of 1 to 5% by weight of the wax, but a gentle decrease in the region of 5% by weight or more.

Table 6 below shows the wax prepared by washing with phosphate after washing in the decolorization process of the above example, the adsorption temperature is 80 ° C., the adsorption time is 60 minutes, the amount of the adsorbent is 5% by weight of the beeswax, and the activated carbon constituting only the adsorbent under vacuum. Only the mixed weight ratio of the activated clay and the decolorization process is performed and the results are shown.

As shown in Table 6, when the mixed weight ratio of activated carbon and activated clay is 50:50, it can be seen that it exhibits the highest decolorizing power.

Table 7 below shows that the mixture weight ratio of activated carbon and adsorbent is 50:50, and the amount of adsorbent is 5 of the input beeswax in the two cases in which the dense wax obtained by the secondary rendering is phosphated and not phosphated. Weight%, adsorption time is 60 minutes, adsorption temperature is 80 ℃, after the decolorization process under vacuum, the results are shown.

As shown in Table 7 above, it can be seen that performing the phosphoric acid treatment process is performed more efficiently the decolorizing process.

Table 8 below shows the sample introduced into the deodorization process after the decolorization and filtration of the above embodiment. At this time, the sample added to the deodorizing process was treated with phosphate and washed with coarse wax, and then the adsorbent having a mixed weight ratio of activated carbon: activated clay was 50:50 was added at 5% by weight of the wax, and the adsorption temperature was 80 ° C. and the adsorption time was 60 Deodorizing process was carried out under 15 different conditions according to pressure, temperature, time, and amount of steam, respectively, as shown in Table 8 below, which was decolorized and filtered under a minute and vacuum.

Table 9 below shows the results after the deodorization process using the sample of Table 8 above.

As shown in Table 9, the analysis result according to the deodorizing temperature was most suitable 200 ~ 250 ℃, the pressure during deodorization showed a better result with a higher vacuum degree, the deodorization time is 2 hours of the amount of beeswax added to the deodorization process It can be seen that the results are good in the range of 5 to 7% by volume / weight (v / w)%.

As described above, the method for producing beeswax according to the present invention is simple for facilities and processes, and is easy for industrial application since there is no risk to human body, and is particularly suitable for the production of beeswax derived from Apis cerana. In addition, when honey producers produce dense bees, they can use small subdivision facilities that separate honey from honeycombs.

Claims (2)

(a) When the beeswax derived from Apis cerana is heated and liquefied, and then the pH is 5 to 6 after stirring by adding 0.05 to 0.5% by weight of a phosphoric acid solution at a concentration of 35 to 45%. Washing with water; (b) 2 to 10 weight of beeswax in which the washed beeswax is in a vacuum state and a mixture of activated carbon and activated clay at a temperature of 70 to 200 ° C. is 45:55 to 55:45 in a decolorization process. Decoloration process to adsorb | suck using%; And (c) deodorizing the decolorized beeswax using a vapor of 2 to 10 vol / wt% of beeswax introduced to the deodorization process at a temperature of 100 to 300 ° C. under a vacuum of 0.3 atmospheres. Beeswax manufacturing method. (a) separating honey from the honeycomb of Apis serana; (b) a step of heating by adding water to the honeycomb remaining after the honey is separated; (c) cooling the mixture obtained by the heating step; (d) separating the solid wax from the cooling step; (e) heating and liquefying said beeswax; (f) adding the liquefied coarse bees to a phosphoric acid solution at a concentration of 35 to 45% by adding 0.05 to 0.5% by weight of the coarse bees and stirring, followed by washing with water until pH 5 to 6; (g) 2 to 10 weight of beeswax in which the washed beeswax is in a vacuum state, and a mixture of activated carbon and activated clay at a temperature of 70 to 200 ° C. is 45:55 to 55:45 in a decolorization process. Decoloration process to adsorb | suck using%; And (h) deodorizing the decolorized beeswax using a vapor of 2 to 10 vol / wt% of beeswax to be introduced into the deodorization process at a temperature of 100 to 300 ° C. under a vacuum of 0.3 atmospheres. Beeswax manufacturing method.

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