WO2018101662A1 - Method for preparing hard capsule and hard capsule prepared thereby - Google Patents

Abstract

The present invention relates to a method for preparing a hard capsule, comprising the steps of: (1) preparing an aqueous composition for a hard capsule by mixing a water-soluble cellulose ether, an alcohol, and water; (2) dipping a mold pin, having been preheated to 35-55°C, in the aqueous composition for a hard capsule, and then recovering the same; and (3) drying the recovered mold pin in a temperature range of 20-55°C. According to the present invention, a high-quality hard capsule can be prepared even if a mold pin preheated to a low temperature of 55°C or lower is used and a drying process at 55°C or lower is carried out, and, resultantly, capsule costs can be reduced by decreasing energy costs.

Description

Method for preparing hard capsules and hard capsules prepared therefrom

The present invention relates to a method for producing hard capsules, and more particularly, to a method for preparing high quality hard capsules at a preheating temperature and a drying temperature of a low mold pin of 55 ° C. or less, and a hard capsule prepared therefrom.

Capsules used in medicine and health functional foods are usually prepared based on gelatin or cellulose ether. Advantages of gelatin capsules include high industrial productivity and price competitiveness, but when the moisture content is 10% by weight or less, plasticity is lost and impact resistance is significantly worsened. In addition, since the use of gelatin is limited due to problems such as mad cow disease, a capsule manufactured using cellulose ether, which is a vegetable material instead of gelatin, is in the spotlight.

On the other hand, there are two types of capsules, a hard type and a soft type. In the case of a hard capsule, a capsule is generally manufactured by a dip molding method using a hot pin process. According to this method, a hard capsule shell is obtained by dipping a mold fin preheated to a high temperature into a film forming composition, recovering the mold fin in a dipping bath to gel the film forming polymer on the mold fin, and then drying the film. It will be prepared. The dried shell is then removed from the mold pin and cut to the desired length to obtain a hard capsule cap and body. And finally, the hard capsule body is filled with powder or granule medicine or health food, and then the hard capsule cap is coupled to the body to complete the final product.

When using this kind of dip forming method, it is necessary to allow the film forming composition to adhere to the fin surface and to gel quickly when the fin is recovered from the dipping bath. This is to produce a capsule having the desired film thickness distribution by preventing the composition from flowing on the fin surface.

As such a conventional method, Patent Document 1 (Domestic Patent Publication No. 10-2009-0057470) (a) has a methoxy content of 27.0 to 30.0%, a hydroxypropoxy content of 4.0 to 7.5% and water at 20 ℃ Providing an aqueous composition comprising HPMC having a viscosity of 3.5 to 6.0 cps as a 2% by weight solution in water; (b) preheating the dipping pin such that the temperature of the dipping pin is 55-95 ° C. when the dipping pin is dipped into the aqueous composition; (c) dipping the preheated dipping pin into the aqueous composition maintained at a temperature between 10 and 1.0 ° C. below the gelation temperature of the aqueous composition; (d) recovering the dipping pins from the aqueous composition to obtain a film on the dipping pins; And (e) drying the film on the dipping pin to obtain a shaped capsule shell on the dipping pin at a temperature higher than the gelation temperature of the aqueous composition. This is described. The method also describes that HPMC capsules with standardized dimensions can be prepared.

Looking at the HPMC hard capsule manufacturing method according to the patent document 1, the dipping pin preheating process of step (b) is in the temperature range of 55 ~ 90 ℃, and the drying process of the step (e) is 50 ~ 90 ℃ temperature range Is performed in In order to perform such a high temperature manufacturing process, the energy cost is excessively spent, which greatly affects the manufacturing cost of hard capsules. In addition, if heat is not correctly transferred to the mold pin or a temperature deviation occurs during drying, a problem may occur in capsule quality.

Therefore, even if the pre-heating and drying process of the mold pin at a low temperature, it is possible to form a high-quality hard capsules to save energy, and to reduce the problems caused by the temperature deviation during drying, and the method for manufacturing hard capsules Research is needed.

[Preceding technical literature]

[Patent Documents]

(Patent Document 1) KR1020090057470 A

The problem to be solved by the present invention is to provide a method for producing a high quality hard capsule at a preheating temperature and a drying temperature of a low mold pin of 55 ℃ or less.

In addition, to provide a hard capsule prepared according to the manufacturing method.

In order to solve the above problems, the present invention comprises the steps of (1) preparing an aqueous composition for hard capsules by mixing a water-soluble cellulose ether, alcohols and water; (2) immersing the mold pin preheated to 35-55 ° C. into the aqueous composition for hard capsules and then recovering; And (3) provides a method for producing a hard capsule comprising the step of drying the recovered mold pin at a temperature range of 20 ~ 55 ℃.

In the step (1), the aqueous composition for hard capsules may be prepared in a temperature range of 10 ~ 25 ℃.

And, it may further comprise the step of aging the aqueous composition for hard capsules prepared according to step (1) for 2 to 12 hours at a temperature range of 10 ~ 25 ℃.

The content of the water-soluble cellulose ether may be 10 to 25% by weight based on 100% by weight of the aqueous composition for hard capsules, and the content of the alcohol may be 10 to 30% by weight.

The water soluble cellulose ether may include at least one selected from the group consisting of hydroxypropyl methyl cellulose (HPMC), hydroxyethyl methyl cellulose (HEMC) and methyl cellulose (MC), wherein the hydroxypropyl methyl cellulose (HPMC) ) May preferably have a methoxyl substitution rate of 19 to 30%, and a hydroxypropoxyl substitution rate of 4 to 8%.

The viscosity of the aqueous solution of 2% by weight of the cellulose ether may be 3 to 15 cps when measured at 20 ° C. under a Ubbelohde viscometer.

The alcohols may include one or more selected from the group consisting of ethanol, methanol, isopropanol and butanol.

In step (3), the drying time may be 1 to 90 minutes.

Step (3) may include a first drying step of drying the mold pin recovered according to step (2) at 40 to 55 ° C. for 1 to 20 minutes; And a second drying step of drying the mold pin after the first drying step for 20 to 90 minutes at 20 to 40 ° C.

In addition, the present invention provides a hard capsule prepared according to the manufacturing method.

According to the present invention, by using a mold pin preheated to a low temperature of 55 ℃ or less, by performing a drying process at 55 ℃ or less to produce a high-quality hard capsules can reduce energy costs, consequently reduce the capsule cost Can be.

In addition, according to the present invention, since the drying process is carried out in a temperature range of 20 ~ 55 ℃ can reduce the temperature deviation that can occur during the drying process compared to the conventional method, thereby reducing the quality degradation problem of the capsule.

1 is a photograph showing a comparison of the hard capsules prepared according to Example 1 and Comparative Example 1.

Figure 2 is a photograph showing a comparison of the hard capsules prepared according to Example 2 and Comparative Example 2.

Figure 3 is a photograph showing a comparison of the hard capsules prepared according to Example 3 and Comparative Example 3.

Figure 4 is a photograph showing a comparison of the hard capsules prepared according to Example 4 and Comparative Example 4.

The present invention comprises the steps of (1) preparing a hard capsule aqueous composition by mixing a water-soluble cellulose ether, alcohols and water; (2) immersing the mold pin preheated to 35-55 ° C. into the aqueous composition for hard capsules and then recovering; And (3) relates to a method for producing a hard capsule comprising the step of drying the recovered mold pin at a temperature range of 20 ~ 55 ℃.

Hereinafter, a step-by-step look at the method for producing a hard capsule according to an embodiment of the present invention.

(1) step of preparing an aqueous composition for a hard capsule

This step is to prepare an aqueous composition for hard capsules by mixing water-soluble cellulose ether, alcohols and water.

In this step, the hard capsule aqueous composition may be prepared in a temperature range of 10 ~ 25 ℃. Specifically, the manufacturing process of the aqueous composition for hard capsules, (a) dispersing the cellulose ether in hot water of 70 ℃ or more, (b) lowering the temperature of the dispersion obtained according to (a) to 50 ~ 60 ℃ And then adding alcohols to dissolve the cellulose ether, and (c) lowering the solution obtained according to the step (b) to 10 to 25 ° C. to obtain an aqueous composition for hard capsules in which cellulose ether is completely dissolved. can do.

The water soluble cellulose ether is the main component of the aqueous composition for hard capsules. The water-soluble cellulose ether is derived from cellulose which is a vegetable material and has an advantage that is harmless to the human body. As used herein, "cellulose ether" means a cellulose derivative in which the hydroxy group of cellulose is etherified using an etherifying agent.

The content of the cellulose ether may be 10 to 25% by weight based on 100% by weight of the aqueous composition for hard capsules. If the content of the cellulose ether is less than 10% by weight, there is a fear that a capsule having a suitable thickness may not be obtained. On the other hand, if the content of the cellulose ether is less than 25% by weight, the viscosity may be excessive and the bubble removal may not be easy.

The water soluble cellulose ether may include at least one selected from the group consisting of hydroxypropyl methyl cellulose (HPMC), hydroxyethyl methyl cellulose (HEMC) and methyl cellulose (MC). In this case, the hydroxypropyl methyl cellulose (HPMC) may preferably have a methoxyl substitution rate of 19 to 30% and a hydroxypropoxyl substitution rate of 4 to 12%.

It is preferable that the 2 weight% aqueous solution viscosity of the said cellulose ether is 3-15cps when measured on 20 degreeC conditions with a Uvelode viscometer. When the viscosity is less than 3 cps, the thickness of the hard capsules may be excessively thin. On the other hand, when the viscosity exceeds 15 cps, there is a fear that workability may be reduced when forming a capsule due to the high viscosity.

The alcohols serve to help the water-soluble cellulose ether to be dissolved in the aqueous composition for hard capsules. The alcohol content may be 10 to 30% by weight based on 100% by weight of the aqueous composition for hard capsules. If the content of the alcohol is less than 10% by weight, there is a fear that the solubility of the cellulose ether is lowered, while if the content of the alcohol exceeds 30% by weight, the evaporation rate of the alcohol in the manufacture of capsules is faster, smooth wrinkles There is a fear that a capsule that could not be obtained. The alcohols may include at least one selected from the group consisting of ethanol, methanol, isopropanol and butanol.

In addition, the method for preparing a hard capsule according to the present invention may further include the step of aging the aqueous composition for hard capsules prepared according to step (1) for 2 to 12 hours at a temperature range of 10 to 25 ℃. .

When the low temperature aging process is further included, bubbles in the aqueous composition for hard capsules may be sufficiently removed, and the aqueous composition for hard capsules having high homogeneity, uniform viscosity, and excellent capsule moldability may be provided. have. Therefore, the aqueous composition for hard capsules subjected to the aging process may be molded using a mold pin preheated to a low temperature, and may also produce hard capsules of excellent quality even if dried at a low temperature.

In this case, when the aging temperature is less than 10 ℃, the viscosity is too high, there is a risk that the capsule film is thick, while when it exceeds 25 ℃ cellulose ether may not be completely dissolved to obtain a homogeneous film.

If the aging time is less than 2 hours, the cellulose ether solution is not fully aged, there is a risk that the bubbles in the solution may not be completely removed, it may be difficult to form the capsule under low preheating temperature and drying temperature, while 12 hours If exceeded, there is a fear that the improvement effect against time will not appear.

(2) mold pin dipping and recovery step

This step is a step of recovering after immersing the mold pin preheated to 35 ~ 55 ℃ into the aqueous composition for hard capsules prepared according to step (1).

The preheating temperature of the mold pin is an important factor in determining the thickness of the capsule. As the temperature is lowered, the thickness of the mold pin can be controlled to be thin. When the temperature is increased, the thickness of the mold can be controlled to be thicker. According to the present invention, by preheating the mold pin to 35 ~ 55 ℃ as described above it is possible to mold the capsule of the desired thickness. This is an effect according to the hard capsule manufacturing method of the present invention, it is possible to reduce the energy cost compared to the conventional method was possible to preform the capsule molding only 55 ℃ ~ 90 ℃ temperature.

This effect may be more pronounced in the case of an aqueous composition for hard capsules, which has undergone a step of aging for 2 to 12 hours in the temperature range of 10 to 25 ℃ described above. Specifically, in the case of the aqueous composition for hard capsules undergoing the aging process, using a mold pin preheated to a low temperature of 55 ℃ or less, even if the drying process described below in a temperature range of 55 ℃ or less uniform film thickness and It is desirable to be able to produce high quality hard capsules with a smooth surface.

If the preheating temperature is less than 35 ℃ is difficult to commercialize because the aqueous composition for hard capsules flow down without being fixed to the mold pin, on the other hand, if the temperature exceeds 55 ℃ excessive energy cost is low economical.

(3) mold pin drying step

This step is a step of drying the recovered mold pin in the temperature range of 20 ~ 55 ℃ according to step (2).

The purpose of drying in this step is to control the flow by reducing the moisture content of the aqueous composition applied to the mold pins. According to the present invention, the above object can be achieved by performing the drying process in a temperature range of 20 to 55 ° C. In addition, as an effect of the hard capsule manufacturing method according to the present invention, it should be dried at a temperature of 55 ℃ or more it is possible to reduce the energy cost compared to the conventional method was fixed without flowing the aqueous composition applied to the mold pin.

If the drying temperature is less than 20 ℃ flow is generated before the applied solution is fixed in the pin does not form a capsule, while if it exceeds 55 ℃ energy cost is excessively low and economic efficiency is low.

The drying time at the drying temperature may be 1 to 90 minutes. If the drying time is less than 1 minute, the applied solution may not be fixed and flow may occur. If the drying time is 90 minutes, the drying proceeds sufficiently and no further drying is necessary.

Alternatively, the drying of the mold pin may include a first drying step of drying the recovered mold pin according to the step (2) at 40 to 55 ° C. for 1 to 20 minutes; And a second drying step of drying the mold pin after the first drying step for 20 to 90 minutes at 20 to 40 ° C.

In the first drying step, when the drying temperature is less than 40 ℃ or the drying time is less than 1 minute, there is a fear that the flow occurs before the applied solution is fixed in the pin may have difficulty in molding the capsule. When the first drying temperature exceeds 55 ° C., the energy cost is excessively low, and the economical efficiency is low. When the first drying time exceeds 20 minutes, the moisture is excessively dried to reduce the moisture in the capsule film within a short time. Cracks may occur in the capsule.

If the drying temperature is less than 20 ℃ or the drying time is less than 20 minutes in the second drying step has a high moisture content is likely to deform the capsule, the drying temperature is more than 40 ℃ or drying time is more than 90 minutes In the case of overdrying, the strength of the capsules may be weakened and cracked due to the low moisture content.

The hard capsules produced by the production method of the present invention show excellent quality similarly to the hard capsules prepared according to the existing methods even under low preheating and drying temperatures of 55 ° C or lower. Therefore, the hard capsule produced by the above production method can be used for various uses, such as pharmaceuticals and health functional food.

Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples.

Example 1

<Preparation of Aqueous Composition for Hard Capsule>

20 wt% of hydroxypropyl methyl cellulose (HPMC, 4.5cps) (Lotte Fine Chemical, BN4) was added and dispersed in 60 wt% of purified water at 80 ° C. After the temperature of the dispersion in which the HPMC was dispersed was lowered to 60 ° C., 20 wt% of ethanol (a large gold, 95%) was added to the dispersion to prepare an HPMC solution. At this time, the substitution rate of the methoxyl group (methoxyl) of the HPMC is 29.2%, hydroxypropoxyl (hydroxypropoxyl) substitution rate is 6.0%. In addition, the viscosity of the HPMC is a value measured under the condition of 20 ° C. using a Ubbelohde viscometer in a 2% by weight aqueous solution.

Subsequently, the HPMC solution was cooled to 15 ° C., and then heated to 25 ° C. and aged for 6 hours to prepare an aqueous composition for hard capsules.

<Preparation of Hard Capsule>

The aqueous composition for hard capsules maintained at 25 ° C. was immersed in a mold pin (prepared by TECHNOPHAR, pin, # 0) preheated at 50 ° C. to apply the aqueous composition to the mold pin.

Thereafter, the mold pins were recovered from the aqueous composition, and dried at 25 ° C. for 5 minutes to prepare hard capsules.

Examples 2-4 and Comparative Examples 1-4

Hard capsules were prepared in the same manner as in Example 1, except that the HPMC, ethanol and purified water, and the preheating temperature and drying temperature of the mold pin were adjusted as described in Table 1 below.

HPMC (wt%) Ethanol (wt%) Purified water (wt%) Preheating temperature (℃) Drying temperature (℃) Example 1 20 20 60 50 25 Example 2 20 20 60 50 50 Example 3 20 20 60 40 25 Example 4 20 20 60 40 40 Comparative Example 1 20 0 80 50 25 Comparative Example 2 20 0 80 50 50 Comparative Example 3 20 0 80 40 25 Comparative Example 4 20 0 80 40 40

1 to 4 are pictures showing the hard capsules prepared according to Examples 1 to 4 and the hard capsules prepared according to Comparative Examples 1 to 4, respectively. 1 to 4, in the case of hard capsules prepared according to Examples 1 to 4, the flowability is appropriate compared to the hard capsules of Comparative Examples 1 to 4 prepared according to the same preheating temperature and the first drying temperature conditions, respectively It can be clearly seen that the capsule is molded stably.

As described above, the embodiments disclosed in the present invention are not intended to limit the technical idea of the present invention but to explain the present invention, and the scope of the present invention should be interpreted by the following claims, and all technical ideas within the scope equivalent thereto. Should be construed as being included in the scope of the present invention.

Claims (11)

(1) mixing the water-soluble cellulose ether, alcohols and water to prepare an aqueous composition for hard capsules; (2) immersing the mold pin preheated to 35-55 ° C. into the aqueous composition for hard capsules and then recovering; And (3) The method of producing a hard capsule comprising the step of drying the recovered mold pin in a temperature range of 20 ~ 55 ℃. The method of claim 1, In the step (1), the hard capsule aqueous composition is a method of producing a hard capsule, characterized in that is produced in a temperature range of 10 ~ 25 ℃. The method of claim 1, The method of producing a hard capsule further comprising the step of aging the aqueous composition for hard capsules prepared according to step (1) for 2 to 12 hours at a temperature range of 10 ~ 25 ℃. The method of claim 1, The content of the water-soluble cellulose ether is 10 to 25% by weight based on 100% by weight of the aqueous composition for hard capsules, the content of the alcohol is a method of producing a hard capsule, characterized in that 10 to 30% by weight. The method of claim 1, The water-soluble cellulose ether is hydroxypropyl methyl cellulose (HPMC), hydroxyethyl methyl cellulose (HEMC) and methyl cellulose (MC) method for producing a hard capsule, characterized in that it comprises one or more selected from the group consisting of. The method of claim 5, The hydroxypropyl methyl cellulose (HPMC) is a methoxyl group (methoxyl) substitution rate of 19 to 30%, hydroxypropoxyl (hydroxypropoxyl) substitution method of the hard capsules, characterized in that 4 to 8%. The method of claim 1, The 2 wt% aqueous solution viscosity of the cellulose ether is a method for producing hard capsules, characterized in that 3 ~ 15cps when measured under the conditions of 20 ℃ by Uvelode viscometer. The method of claim 1, The alcohol is a method of producing a hard capsule, characterized in that it comprises at least one selected from the group consisting of ethanol, methanol, isopropanol and butanol. The method of claim 1, The drying step of step (3) is a method for producing hard capsules, characterized in that for 1 to 90 minutes. The method of claim 1, The drying step of the step (3) is a first drying step of drying for 1 to 20 minutes at 40 ~ 55 ℃; And a second drying step of drying at 20 to 40 ° C. for 20 to 90 minutes. Hard capsules prepared according to any one of claims 1 to 10 manufacturing method.

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