KR101080444B1 - Manufacturing method of water-soluble gel having cooling effect - Google Patents

Abstract

The present invention relates to a method for preparing a water-soluble gel, and in particular, by mixing a poorly soluble menthol component with a water-soluble gel without using an organic solvent, the manufacturing cost is reduced, the spreadability of the gel is improved, and the stickiness is removed to improve the quality. In addition, the present invention relates to a method for preparing a water-soluble gel having a cooling effect by increasing the cooling effect by mixing volatile components such as ethanol, isopropanol, butyl alcohol, and the like.

Water Soluble Gel, Cooling Effect, Menthol, Sports Massage Gel, Ultrasonic Gel

Description

Manufacturing method of water-soluble gel having cooling effect

The present invention relates to a method for preparing a water-soluble gel, and in particular, by mixing a poorly soluble menthol component with a water-soluble gel without using an organic solvent, the manufacturing cost is reduced, the spreadability of the gel is improved, and the stickiness is removed to improve the quality. In addition, the present invention relates to a method for preparing a water-soluble gel having a cooling effect by increasing the cooling effect by mixing volatile components such as ethanol, isopropanol, butyl alcohol, and the like.

Water-soluble gels, unlike fat-soluble gels, suspensions and creams, can be easily absorbed by the skin and are not sticky after being applied. They are also easily washed with water and used as sports massage gels.

However, in order to use such a water-soluble gel as a sports massage gel, it was necessary to include analgesic and anti-inflammatory components such as menthol and camphor, which have analgesic and anti-inflammatory effects, in the water-soluble gel.

However, since such menthol, camphor, and the like are not water-soluble or poorly water-soluble, they are used in a polyhydroxy alcohol-based organic solvent.

For example, according to the applicant's patent registration No. 461049, in order to solve such poor solubility of menthol, a method of dissolving menthol using polyhydric polyhydric alcohol such as glycerin or propylene glycol was used.

However, excessive mixing of polyhydric alcohols such as glycerin or propylene glycol not only increases the cost of the gel, but also reduces the quality of the gel. Too much polyhydric alcohols, such as glycerin or propylene glycol, can cause the gel to become sticky and the polyhydric alcohols with menthol dissolved in the crosslinked gel can be easily separated. In order to solve this problem, an inorganic thickener such as SiO 2 may be used, which causes the gel to aggregate and degrades the gel, thereby degrading the quality.

The present invention was invented to solve the above-mentioned problems of the prior art, and the present invention is to reduce the manufacturing cost, improve the spreadability of the gel and remove the stickiness by mixing the poorly soluble menthol component in the water-soluble gel without using an organic solvent The purpose of the present invention is to provide a method of preparing a water-soluble gel having a cooling effect by improving the quality and further increasing the cooling effect by mixing volatile components such as ethanol, isopropanol, butyl alcohol, and the like.

The water-soluble gel having a cooling effect according to the present invention is characterized in that it comprises 0.1 to 3.0% by weight of thickener, 0.1 to 13% by weight of menthol or DL-campa and a residual amount of water.

According to another preferred feature of the present invention, the water-soluble gel having a cooling effect is further included 0.01 to 0.5% by weight parabens preservative.

According to another preferred feature of the present invention, the water-soluble gel having a cooling effect is further included 1 to 70% by weight of volatiles.

According to another preferred feature of the invention, the volatile substance is at least one of ethanol, isopropyl alcohol or butyl alcohol.

According to another preferred feature of the present invention, the water-soluble gel having a cooling effect is further included 0.01 to 3% by weight of a moisturizer.

According to another preferred feature of the invention, the thickener is carboxyvinyl polymer, sodium polyacrylate, polyvinyl acetal diethylamino acetate, polyvinyl alcohol, polyvinylpyrrolidone, methacrylic acid-ethyl acrylate copolymer, methacrylic acid- At least one selected from the group consisting of an ethyl methacrylate copolymer, an ethyl methacrylate-trimethylammonium ethyl chloride copolymer, and a dimethylaminoethyl methacrylate-methyl methacrylate copolymer.

According to another preferred feature of the invention, the thickener is ethyl cellulose, carboxymethyl cellulose and salts thereof, carboxymethylethyl cellulose and salts thereof, carboxymethyl starch and salts thereof, croscarmellose and salts thereof, crystalline cellulose, acetic acid At least one selected from the group consisting of cellulose, cellulose acetate cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropylmethyl cellulose, hydroxypropylmethyl cellulose phthalate, powdered cellulose, methylcellulose and methylhydroxypropyl cellulose.

According to another preferred feature of the invention, the thickener, gum arabic, carrageenan, galactan, agar, quince seed gum, guar gum, tragacanth rubber, pectin, met, locust bean gum, wheat starch, rice starch, Corn starch, potato starch, cran, xanthan gum, succinoglucan, textan, hyaluronic acid, pullulan, aloe vera, albumin, casein, collagen, gelatin, fibroin.

According to another preferred feature of the invention, the thickener is pregelatinized starch, partially pregelatinized starch, carboxymethyl starch, dextrin, methyl starch, sodium alginate, propylene glycol ester, sodium chondroitin sulfate, sodium hyaluronate, hydrous dioxide At least one selected from the group consisting of silicon, light silicic anhydride, colloidal alumina, bentonite, and laponite.

Method for producing a water-soluble gel having a cooling effect according to the present invention is a polymer hydration step of preparing a polymer material by adding a thickener 0.1 to 3.0% by weight in a residual amount of water and stirring at high speed; Liquid phase dissolving menthol or DL-campa at 43-216 ° C. to a liquid state; 0.1-3% by weight of the polymer material prepared in the polymer hydration step and 0.1-13% by weight of the liquid menthol or DL-campa prepared in the liquid phase manufacturing step, and the high-speed stirring in the state that the menthol or DL-campa do not precipitate A mixing step of preparing a mixture in which the polymer material and analgesic component are dispersed; It characterized in that it comprises a gelling step of gelling the mixture prepared in the mixing step.

According to another preferred feature of the invention, when the thickener is a carboxyvinyl polymer, the gelling step is gelled by adding 0.03 to 3% by weight of an alkaline solution to the mixture prepared in the mixing step.

According to another preferred feature of the present invention, in the polymer hydration step, 1 to 70% by weight of any one or more volatiles of ethanol, isopropyl alcohol or butyl alcohol is further added to the water and stirred at high speed.

According to another preferred feature of the present invention, in the polymer hydration step, the addition of 0.01-0.5% by weight of paraben preservatives to the water is stirred at high speed.

According to another preferred feature of the present invention, in the polymer hydration step, the addition of 0.01-3% by weight of a moisturizer to the water is stirred at high speed.

According to another preferred feature of the invention, the mixing step proceeds at a temperature of 43-82 ° C.

The water-soluble gel having a cooling effect according to the present invention solves the problems caused by excessive use of organic solvents of polyhydric alcohols such as glycerin or propylene glycol, thereby reducing the cost of the gel, improving the spreadability of the gel, and eliminating stickiness. Much improved.

In addition, it is conveniently mixed with volatile alcohols such as ethanol or isopropanol, which gives a cooling effect. The water-soluble gel with the cooling effect can be maximized by the cryotherapy of the gel with the therapeutic effect of the ultrasonic wave itself, especially in the physiotherapy using ultrasound, which has no choice but to use the water-soluble gel.

In general, the water-soluble gel is a gelling agent is mixed with an appropriate amount of thickener in water to form a gel with a high viscosity while causing a crosslinking reaction. These water-soluble gels are prepared by mixing an appropriate amount of menthol as an analgesic ingredient derived from natural extracts having analgesic and anti-inflammatory effects to prepare a water-soluble gel having an analgesic anti-inflammatory effect of menthol, gels for physiotherapy, gels for treating joints and muscle pain or sports Can be used as a massage gel.

The problem is that menthol is difficult to mix in conventional water soluble gels with both water insoluble or poorly water soluble materials.

Therefore, in the present invention, instead of dissolving the analgesic component in a polyhydric alcohol-based solvent such as glycerin or propylene glycol as in the prior art, it solves the problem through the method of making the analgesic component in liquid form directly at a temperature of 43 ° C. or higher and mixing it into a conventional water-soluble gel. It was.

Hereinafter, the present invention will be described in more detail.

The water-soluble gel having a cooling effect according to the present invention contains 0.1 to 3.0% by weight of thickener, 0.1 to 13% by weight of menthol or DL-campa and residual amount of water.

In addition, parabens preservatives may be further added in an amount of 0.01 to 0.5% by weight for preservation of the water-soluble gel according to the present invention.

In addition, 1 to 70% by weight of volatiles may be additionally included to further increase the cooling effect.

In addition, the water-soluble gel according to the present invention may further contain 0.01 to 3% by weight of glycerin or propylene glycol to give a moisturizing effect.

Hereinafter, a method for preparing a water-soluble gel according to the present invention will be described in detail.

The method for preparing a water-soluble gel according to the present invention includes a polymer hydration step, a liquid phase production step, a mixing step, and a gelation step. Each step will be described in detail below.

In the polymer hydration step, a thickener is added to water, followed by hydration by stirring at high speed for several hours.

As the thickener of the present invention, a synthetic polymer, carboxyvinyl polymer (carbopol), sodium polyacrylate, polyvinyl acetal diethylamino acetate, polyvinyl alcohol, polyvinylpyrrolidone, methacrylic acid-ethyl acrylate copolymer, methacrylic acid-meta Ethyl acrylate copolymer, ethyl methacrylate-methacrylate trimethylammonium ethyl copolymer, and dimethylaminoethyl methacrylate-methyl methacrylate copolymer.

Cellulose polymers in the semi-synthetic polymer as the thickener of the present invention include ethyl cellulose, carboxymethyl cellulose and salts thereof, carboxymethylethyl cellulose and salts thereof, carboxymethyl starch and salts thereof, croscarmellose and salts thereof, crystalline cellulose, cellulose acetate Cellulose acetate, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropylmethyl cellulose, hydroxypropylmethyl cellulose phthalate, powdered cellulose, methylcellulose, methylhydroxypropyl cellulose, and the like.

Natural polymers used as thickeners of the present invention include gum arabic, carrageenan, galactan, agar, quince seed gum, guar gum, tragacanth rubber, pectin, mannan, locust bean gum, wheat starch, rice starch, corn starch, Potato starch, cadmium, xanthan gum, succinoglucan, textan, hyaluronic acid, pullulan, aloe vera, albumin, casein, collagen, gelatin, fibroin and the like.

The semisynthetic polymer used as the thickener of the present invention may include pregelatinized starch, partially pregelatinized starch, carboxymethyl starch, dextrin, methyl starch, sodium alginate, propylene glycol ester, sodium chondroitin sulfate, sodium hyaluronate and the like. Examples of the inorganic substance used in the thickener of the present invention include hydrous silicon dioxide, hard silicic anhydride, colloidal alumina, bentonite, and laponite.

Thickeners use 0.1 to 3 weight percent. If the thickener is less than 0.1% by weight, the gel may be too thin to flow through the skin, and if the thickener is more than 3% by weight, the viscosity of the gel may be too high to reduce spreadability.

The water-soluble gel in the present invention can feel a refreshing feeling by the menthol component, but may be used by mixing the volatile components with water to give a more cooling effect. Here, the volatile component lowers skin temperature and promotes crystallization (Crystallization) of menthol present in the molecular state in the gel because the water-soluble gel according to the present invention takes away the heat of vaporization while vaporizing from the skin when applied to the skin. Here, too, crystallization energy is consumed, resulting in a lower temperature. As these vaporization energy and crystallization energy interact, it lowers the temperature of the skin and gives a dual cooling effect. The water-soluble gel with the cooling effect (Cryotherapy) is added to the gel during the physiotherapy using ultrasound can maximize the physical therapy by synergistic effect and the therapeutic effect of the ultrasound itself. Water-soluble gel with this cooling effect is also suitable as a gel for treating joint pain, muscle pain or sports massage. Specific examples of the volatile components include any one or more of ethanol, isopropyl alcohol or butyl alcohol, which are mixed at a ratio of 1 to 70% by weight. If it is less than 1% by weight, there is little cooling effect due to insufficient vaporization effect, and if it exceeds 70% by weight, the gel is too thin due to the influence on the physical properties of the gel.

The water uses deionized water and is stirred at high speed for several hours until all the polymers are hydrated.

In addition, it is preferable that the water-soluble gel according to the present invention further contains 0.01 to 0.5% by weight of parabens preservative for preservation. Examples of parabens preservatives include methyl paraoxybenzoate and propyl paraoxybenzoate, and less than 0.01% by weight of the preservatives may be less effective in the growth of fungi, and when the amount exceeds 0.5% by weight, the preservatives may irritate the skin. have. Paraben preservatives are put together in water and stirred at high speed.

In addition, the water-soluble gel according to the present invention may further include a moisturizing agent for a moisturizing effect. Examples of the moisturizing agent include glycerin or propylene glycol, and these preferably contain 0.01 to 3% by weight. If it is less than 0.01% by weight, there is almost no moisturizing effect, and if it exceeds 3%, there is a problem of dissolving menthol in the gel and separating from the gel. Moisturizing glycerin and propylene glycol may be added before the water-soluble gel according to the present invention is formed and stirred at high speed. For example, it can be put together with water in a polymer hydration step and agitated at high speed.

In the liquid phase manufacturing step, the analgesic component is heated to a temperature above the melting point to form a liquid state. In the present invention, as an analgesic component, menthol or DL-campa, which are natural extracts having analgesic and anti-inflammatory effects, may be used, and among them menthol, L-menthol is more preferably used. These analgesic ingredients not only have antibacterial, anti-inflammatory and soothing effects, but also have a refreshing scent and refreshing feeling. In this case, the menthol is used in the range of 0.1 to 13% by weight, respectively, does not cause side effects on the skin or human body, and if less than 0.1% by weight, there is no pharmacological effect or cooling effect. There is. The menthol component maximizes the refreshing feel of the water-soluble gel according to the present invention together with the volatile components described above.

Since the analgesic component such as menthol or die-campa is not directly dissolved in the water-soluble gel, in the present invention, after the analgesic component such as menthol or die-campa is heated to a melting point or higher in a liquid state, the above-described polymer hydration step It is subjected to a process of high speed agitation and dispersion in the hydrated polymer mixture. To this end, in the liquid manufacturing step, menthol is dissolved at 43-216 ° C. to a liquid state. If it is less than 43 ℃ menthol does not melt well, if it exceeds 216 ℃ there is a problem menthol vapor occurs.

In the mixing step, 0.1 to 13% by weight of the menthol component of the liquid prepared in the liquid phase preparation step is stirred with high-molecular mixture of 0.1 to 3 wt% of the polymer material prepared in the polymer hydration step, thereby analgesing with the polymer / alcohol / water-aqueous solution. Sufficient dispersing of the components. At this time, if the temperature of the polymer / water / alcohol aqueous solution is too low or the time is too long until the alkaline solution is added to gel, menthol may precipitate. Therefore, the temperature of the aqueous solution should be maintained or gelated quickly. In other words, the menthol or DL-campa component should proceed without precipitation. It is preferable to maintain the temperature of 43-82 degreeC preferably. If the temperature is less than 43 ° C., the menthol may be precipitated if the gelling is not performed quickly. If it is over 82 ° C., the isopropyl alcohol may be vaporized.

The gelation step is a step of gelling the mixture of the polymer / alcohol / water-aqueous solution and analgesic components prepared in the mixing step. This may be accomplished by gelling in accordance with the thickener used. That is, gelation is carried out using a crosslinking agent or hydrolysis. For example, if the thickener is a semi-synthetic polymer of cellulose or natural thickener, it can be gel simply by dissolving in water, and if polyvinylpyrrolidone can be gelled by irradiating with gamma rays.

In particular, when the thickener is a carboxyvinyl polymer (Carbopol), the polymer / water / alcohol mixture containing molten menthol is gelled by adding 0.03 to 1% by weight of an alkaline solution with high speed stirring. Alkaline solution crosslinks by carbopol hydrolysis reaction, about 1 / 3wt% of carbopol amount is used. Here, a crosslinking reaction occurs by undergoing a neutralization step with an alkaline solution, thereby preparing a water-soluble gel according to the present invention. The alkaline solution is for neutralizing acidic Carbopol, and may be used such as amine, ethanolamine, alkali metal hydroxide, ammonium hydroxide, caustic soda or potassium hydroxide. Soda may be most preferably used. When an alkaline solution is added, a uniform gel is formed.

The gel prepared by the above method was observed that the menthol is no longer precipitated or separated at room temperature, but remains 'trapped' in a crosslinked network of polymer / water / alcohol of the gel. It can be explained that the gelling enthalpy of the thickener is sufficiently large that menthol is stably trapped in a molecular state without precipitation in the network of water-alcohol-polymer.

Example 1

35 wt% isopropanol was mixed with deionized water. 1 wt% Carbopol was mixed thereto and rapidly dispersed until hydrated. After stirring for several hours, a homogeneous polymer / water / alcohol mixture was obtained.

This mixture was kept at 43 ° C.

2 wt% of menthol was dissolved at a temperature of 43-100 ° C. The melted elmenthol was mixed with the polymer / water / alcohol solution while stirring at high speed. 0.3 wt% caustic soda aqueous solution was slowly added. Crosslinking occurred and suddenly a uniform water-soluble gel was formed.

Comparative Example 1

In the same manner as in Example 1, the polymer / water / alcohol mixture was hydrated by high-speed stirring, and left at room temperature. 2 wt% of menthol dissolved at 43 ° C. was added thereto, followed by high speed stirring. 0.3 wt% caustic soda solution was added to crosslink to obtain a gel, but it was observed that menthol precipitated through the gel.

Comparative Example 2

2 wt% of menthol was dissolved in 5 wt% of glycerin. This glycerin solution was hydrated in the same manner as in Comparative Example 1 to prepare a polymer / water / alcohol mixture, and 0.5 wt% SiO2 was added as an inorganic thickener. This is to keep the glycerol dissolved in the menthol separated from the gel. Elmentol was mixed with the dissolved glycerin solution and the polymer / SiO 2 / water / alcohol mixture under stirring. Aqueous sodium 0.3 wt% aqueous solution was added to form a water-soluble gel.

division Example 1 Comparative Example 2 Cooling effect Great Great Cooling Effect Duration More than 4 hours 4 hours or less Spreadability from the skin Great Bad Separation of Gels and Solvents Not separated Detached Sticky none has exist

The experiment was checked by item targeting 20 people as a sensory evaluation.

* Cooling effect

After applying gel on the back of each experimenter, the satisfaction of the cooling effect was examined, and when the satisfaction was over 60%, the satisfaction was excellent when the satisfaction was 60% or 40%.

l duration

After applying gel to the back of each experimenter, the average time was calculated after measuring the duration of cooling effect.

* Spread from the skin

After applying gel on the back of each tester's hand, the satisfaction of spreading in the skin was investigated, and when the satisfaction was over 60%, the satisfaction was excellent when the satisfaction was 60% or 40%.

* Separation of Gels and Solvents

After applying gel to the back of each experimenter was observed whether the separation of the gel and the solvent, not separated when not separated more than 60% / less than 60%.

* Sticky

After applying gel on the back of each experimenter, the satisfaction of stickiness was examined, and when the satisfaction was over 60%, the satisfaction was excellent when the satisfaction was 60% or 40%.

In Comparative Example 1, menthol was deposited on the entire gel during the manufacturing process and thus could not be used as a product.

As shown in the above experimental results, Example 1 does not contain an organic solvent component compared to Comparative Example 2 has excellent spreadability in the skin, no stickiness, no separation of the gel and solvent, and also has a cooling effect It lasted more than 4 hours.

Claims (15)

A polymer hydration step of preparing a polymer material by adding 0.1 to 3.0% by weight of a carboxyvinyl polymer, which is a synthetic polymer, into a residual amount of water and stirring at a high speed; Liquid phase dissolving menthol or DL-campa at 43-216 ° C. to a liquid state; 0.1-3% by weight of the polymer material prepared in the polymer hydration step and 0.1-13% by weight of the liquid menthol or DL-campa prepared in the liquid phase manufacturing step, and the high-speed stirring in the state that the menthol or DL-campa do not precipitate Mixing step of preparing a mixture; Method for producing a water-soluble gel having a cooling effect, characterized in that it comprises a gelling step of gelling the mixture prepared in the mixing step. The method of claim 1, wherein the gelling step is gelling by adding 0.03 to 3% by weight of an alkaline solution to the mixture prepared in the mixing step. The water-soluble gel having a cooling effect according to claim 1, wherein 1 to 70% by weight of any one or more volatile substances of ethanol, isopropyl alcohol or butyl alcohol is further added to the water in the polymer hydration step. Manufacturing method. [Claim 2] The method of claim 1, wherein, in the polymer hydration step, 0.01-0.5% by weight of a parabens preservative is added to the water and stirred at a high speed to prepare a water-soluble gel having a cooling effect. The method of claim 1, wherein in the polymer hydration step, 0.01-3% by weight of a moisturizer is additionally added to the water and stirred at high speed. The method of claim 1, wherein the mixing step is performed at a temperature of 43-82 ° C. delete delete delete delete delete delete delete delete delete