KR20010027020A - Method for producing half-coated zeolite and nonaqueous exothermic cosmetics containing the same - Google Patents

Abstract

PURPOSE: A manufacturing process for semi-coated zeolite is provided, which controls absorption rate by improving a part of surface of zeolite, so maintains effects of the heat-sense by heat of hydration of zeolite. A non-water systemic exothermic cosmetics containing same is also provided, which makes skin to be clean, smooth, and elastic. CONSTITUTION: The manufacturing process for semi-coated zeolite is comprised of: (1) dispersing methylhydrogen polysiloxane 0.01-10wt., cyclomethicone 0.01-5wt., and active silane(e.g., N-(β -aminoethyl)-γ-aminopropyltrimethoxysilane) 0.01-10wt. in an organic solvent(mixing ratio between methylhydrogen polysiloxane and cyclomethicone is 1:4-4:1); (2) adding active zeolite(zeolite 3A, 4A, 5A with large heat-generation power) 1-50wt. to (1); (3) heating (2) to 90-150deg.C to get the semi-coated zeolite. The non-water systemic exothermic cosmetics contains the semi-coated zeolite 0.5-60wt., which can be prepared in the form of cleansing masks, cleansing packs, massage packs.

Description

Method for producing semi-coated zeolite and non-aqueous exothermic cosmetics containing the same {Method for producing half-coated zeolite and nonaqueous exothermic cosmetics containing the same}

The present invention relates to a method for preparing a semi-coated zeolite and a non-aqueous exothermic cosmetic containing the same, and more particularly, by modifying a part of the surface of the zeolite, which has a strong absorbing power, by adjusting the moisture absorption rate to maintain the warming effect due to the heat of hydration of the zeolite. The present invention relates to a method of preparing a semi-coated zeolite and a non-aqueous exothermic cosmetic containing the same.

Conventionally, methods for promoting metabolism and easily removing wastes by imparting warmth to the cosmetics, and introducing methods having high calorific value and safe substances into the cosmetics to enhance drug permeability.

For example, Japanese Patent Application Laid-Open No. Hei 4-89424, European Patent No. 187,912, and US Patent No. 3,250,680 describe exothermic cosmetics using heat of hydration of zeolite. However, the above inventions have the disadvantage that they may cause skin burns due to the instantaneous heating of the zeolite. In addition, when a large amount of zeolite is mixed in order to maintain warmth, it is difficult to manufacture a cosmetic and there is a problem in that it is impossible to evenly disperse the zeolite evenly in a manufacturing process.

In particular, U.S. Patent No. 4,626,550 and European Patent No. 187,912 make zeolites by a simple operation such as dehydration, such as a method of making zeolites more difficult to adsorb nitrogen in the atmosphere by ion-exchanging the zeolites, and thus maintaining a calorific value. A method of activation is described.

However, active zeolites generate heat in a short time when reacted with water, so it is difficult to expect a continuous heating effect.

In this regard, US Patent No. 4,379, 143 to which PEG-400 is added is an invention for improving heat storage and achieving a continuous exothermic effect. In addition, Japanese Patent Application Laid-Open Nos. 6-100411, 8-59455, and 6-80534 disclose a base containing polyol insoluble polymer and polyethylene glycol, and these inventions use a hydrophilic medium and a polymer. Thus, when the base and water are in contact with each other, the exothermic reaction is continued by a competition reaction between the zeolite and the polymer.

However, the inventions are insufficient to provide a continuous warmth to the skin due to insufficient heat sustaining effect. In order to compensate for these disadvantages, a method of controlling the strong hygroscopicity of the zeolite has been needed.

The present inventors have found that by appropriately combining methylhydrogen polysiloxane and volatile cyclomethicone to coat the zeolite, the hydration rate of the zeolite can be slowed down by controlling the degree of surface coating of the zeolite.

As a technique for coating silicon, there is a method of simply applying a silicone resin and then drying it to impart fluidity to particles and dispersing silicon having hydrogen directly bonded to silicon to impart water repellency. Japanese Laid-Open Patent Publication No. 70-18999 discloses a method in which dimethyl polysiloxane or methylhydrogen polysiloxane is dissolved in an organic solvent and then contacted / adhered using zinc octate as a catalyst.

However, these methods are different from the silicone coating method used in the present invention. That is, these inventions provide a tool for maximizing the water repellency of the inorganic powder, but there is no method for easily adjusting the coating degree to adjust the degree of coating so that the hygroscopicity can be controlled rather than the complete water repellency.

The present inventors adsorb and coat a mixture of methylhydrogen polysiloxane and cyclomethicone on the zeolite surface in a dispersion system in which methylhydrogen polysiloxane and cyclomethicone are mixed at a constant ratio by a water-repellent coating method to be applied to the powder. In the drying process, a method of preparing a semi-coated zeolite that can control the hygroscopicity by controlling the degree of water repellent coating by volatilizing a micromethicone having a volatility to form a non-coated surface having a predetermined ratio on the zeolite surface.

In addition, the present inventors have completed the present invention by discovering that the result of mixing the anti-coating zeolite with the non-aqueous exothermic cosmetic is that the rate of hydration is controlled to extend the exothermic persistence.

It is an object of the present invention to provide a coating method for semi-coating zeolites with methylhydrogen polysiloxane, cyclomethicone and active silane under non-aqueous conditions.

In addition, an object of the present invention is to provide a non-aqueous exothermic cosmetic containing a semi-coated zeolite using the semi-coating method.

In order to achieve the above object, the present invention provides a method for producing a water-repellent semi-coated zeolite comprising the following steps:

(1) dispersing 0.01-10 weight of methylhydrogen polysiloxane, 0.01-5 weight of cyclomethicone and 0.01-10 weight of active silane in an organic solvent;

(2) adding 1-50 weight of the active zeolite to the reaction obtained in (1); And

(3) warming to temperature 90-150 ° C.

The present invention also provides a non-aqueous exothermic cosmetic containing 0.5-60 weight of the semi-coated zeolite prepared by the above process in order to achieve the above object.

Organic solvents used in the method for preparing a semi-coated zeolite of the present invention include isopropyl alcohol, anhydrous ethanol, anhydrous methanol and the like.

The average molecular weight of methylhydrogen polysiloxane used in the present invention is 1,500-2,500, and the content thereof is preferably 0.01-10 weight. If it exceeds 10 weights, it will become completely water repellent and it is unpreferable.

Micromethicone, which is a volatile silicone, may use tetramers or pentamers, but it is more preferable to use tetramers having a low volatility point in consideration of volatility when drying in the final step.

The mixing ratio of methylhydrogen polysiloxane and cyclomethicone is preferably 1: 4-4: 1. If the ratio is exceeded, it is completely coated and the hygroscopicity cannot be adjusted.

Active silanes include N- (β-aminoethyl) -γ-aminopropyltrimethoxysilane.

The shape of the zeolite to be coated is not particularly limited, but activated zeolites 3A, 4A, and 5A are preferred because they must be exothermic when hydrated. In addition, an improved zeolite in which some of the metal ions are exchanged with K and Ca may also be used, and dehydrated and activated to increase the calorific value. On the other hand, other active zeolites can be used as long as they do not contradict the object of the present invention.

Exothermic cosmetics to which the anti-coating zeolite according to the present invention can be applied include a cleaning mask, a cleaning pack, a massage pack, and the like.

Hereinafter, although an Example is given and the effect of this invention is demonstrated in detail, it is not limited to these Examples.

(Example 1)

According to each composition shown in Table 1 was prepared a water-repellent coating zeolite.

To 50 g of isopropyl alcohol, methylhydrogen polysiloxane, N- (β-aminoethyl) -γ-aminopropyltrimethoxysilane, and cyclomethicone were added and uniformly dispersed. Since the active zeolite and kaolin as a supplement was added and dispersed. After the dispersion was completed, isopropyl alcohol was recovered by a filter, and the prepared zeolite was dried in a drying oven at 90-150 ° C. After drying, the large particle size was pulverized to select only sizes of 100 μm or less.

Ingredient (g) Invention 1 Invention 2 Invention 3 Comparative product 1 Comparative product 2 Comparative product 3 Methylhydrogen Polysiloxane 0.8 0.5 0.2 - 0.5 0.2 Active silane 0.1 0.1 0.1 - 0.1 0.1 Cyclomethicone 0.2 0.5 0.8 One - - Activator 47.8 47.8 47.8 47.8 47.8 47.8 kaoline 1.1 1.1 1.1 1.2 1.6 1.9

Using a semi-coated zeolite prepared in Example 1 to prepare a cleaning mask according to the composition of Table 2. ingredient() Prescription 1 Prescription 2 Prescription 3 Prescription 4 Prescription 5 Prescription 6 Invention 1 30 - - - - - Invention 2 - 30 - - - - Invention 3 - - 30 - - - Comparative product 1 - - - 30 - - Comparative product 2 - - - - 30 - Comparative product 3 - - - - - 30 glycerin 69.7 69.7 69.7 69.7 69.7 69.7 cellulose 0.3 0.3 0.3 0.3 0.3 0.3

The degree of hygroscopicity was determined by measuring the exothermic temperature by time using an infrared camera (Azema, THV470) to determine the delay of hydration with the prepared cosmetics. The measurement was carried out in a chamber at 30 ° C. and a relative humidity of 75, and the humidity and temperature control were controlled using a warm air and a humidifier.

Samples were taken 3g each and thinly coated on the acrylic plate to a thickness of about 0.1mm using a glass plate.The six samples were placed on the same acrylic plate, and the image file was converted into a temperature on a computer by storing an image of heat generated by moisture absorption in an infrared camera. By hour. The results are shown in Table 3.

Prescription 1 (℃) Prescription 2 (℃) Prescription 3 (℃) Prescription 4 (℃) Prescription 5 (℃) Prescription 6 (℃) first 30 30.1 30 30 30 30 1 minute later 31 32 32 35.3 35 37.8 2 minutes later 30.2 33.5 34.5 41 33.2 35.4 3 minutes later 31 34 36 40.1 32 33.3 4 minutes later 32.5 34.5 38 38.7 31 31.1 5 minutes later 34 35 38.7 37 31 31 6 minutes later 34 36 40 37 31.5 31.2 7 minutes later 35 37 40.3 36.5 30.5 31 8 minutes later 36.5 37.5 40.1 36 30.2 30.5 9 minutes later 36 38.1 41 36.1 30.4 30.5 10 minutes later 37 39 40 35.2 30 30.4 11 minutes later 37.8 39.5 39.7 35.4 30 30 12 minutes later 39.8 40 38 35 30.1 30.3 13 minutes later 40 39.8 37 34 30 30 14 minutes later 40.1 39.4 37 34 30.1 30 15 minutes later 40 39.2 37.4 34.2 30 30 16 minutes later 39.7 38 36.5 34 30 30 17 minutes later 37 37.2 36 33.5 30 30.1 18 minutes later 37.4 37 35.3 33 30.1 30.1 After 19 minutes 35.8 36 34 32 30 30 20 minutes later 36 36.2 33 31 30 30

As can be seen from Table 3, the exothermic duration was different according to the degree of the semi-coated zeolite, and the duration of the present invention in the order of 1, 2, and 3 of the present invention was delayed from 8 to 14 minutes compared to general zeolite. It became.

In addition, Comparative Products 2 and 3, which did not use the cyclomethicone used as the anti-coating regulator, did not delay the exotherm time despite the different concentrations of methylhydrogen polysiloxane. In comparison products 2 and 3, the total calorific value was lowered by about 5-7 ° C. compared with the present invention, which was caused by the partial absence of a uniform coating on the whole powder due to the absence of the micromethicone coating agent. This is due to the result of making a fully water repellent zeolite.

(Example 3)

In order to measure the water repellency of the semi-coated zeolite itself, the sedimentation rate was measured by dispersing it in water in the ratio of Table 4. The results are shown in Table 5.

The sedimentation rate was measured as a time when the suspended solids of the coated zeolite suspended in the upper layer disappeared completely as an index of the velocity.

ingredient() Test tube 1 Test tube 2 Test tube 3 Test tube 4 Test tube 5 Test tube 6 Invention 1 30 - - - - - Invention 2 - 30 - - - - Invention 3 - - 30 - - - Comparative product 1 - - - 30 - - Comparative product 2 - - - - 30 - Comparative product 3 - - - - - 30 PEG-7glyceryl Cocoade 0.5 0.5 0.5 0.5 0.5 0.5 Purified water 69.5 69.5 69.5 69.5 69.5 69.5

division Test tube 1 Test tube 2 Test tube 3 Test tube 4 Test tube 5 Test tube 6 Minutes 29 21 11 One - -

As can be seen from the results of Table 5, the invention 1 was the most half-water-repellent coating was a slow sedimentation rate, the order was the order of inventions 2, 3 in the order of coating degree.

Zeolites coated with volatile micromethicones settled fastest and were not coated, and the micromethicones used as coating modifiers did not function as coatings.

In Comparatives 2 and 3, which did not contain the semi-coating regulator micromethicone in the process, some fully water-repellent coating zeolites which did not settle over time continued to float. As a result, it was found that Comparative Products 2 and 3, which did not use the microcoating agent, which was a semi-coating regulator, were completely water-repellent coatings that were biased to some zeolites. In the end, it was found that the cyclomethicone acted as a regulator of the semi-water repellent coating.

(Example 4)

Sensory evaluation was performed on 30 women with the non-aqueous pyrogenic cosmetic prepared in Example 2 to question the duration of fever. The results are shown in Table 6.

In the sensory evaluation, 4g of each product was massaged on both cheeks, and then the feeling of fever was checked.

Prescription 1 () Prescription 2 () Prescription 3 () Prescription 4 () Prescription 5 () Prescription 6 () High calorific value 84.7 82 88.4 89.4 12.1 13.2 Good heat dissipation 91.5 84.3 80.2 22.1 12 13.4 We are satisfied with a feeling of heat 90.3 88.4 82 55.4 32.4 33.7

From the results of Table 6, the exothermic sustainability of the formulations 1, 2, and 3, which contain the semi-coated zeolite, was much higher than that of the non-coated zeolite.

From the calorific value and the exothermic persistence, it was found that half-coated with 0.3% methylhydrogen polysiloxane was excellent.

The present invention provides a non-aqueous exothermic cosmetic that continuously generates heat by making a repellent coating zeolite so that it can be slowly hydrated, thereby providing continuous low-temperature warmth to the skin to promote blood circulation and clean skin, resulting in a clean and smooth effect. It allows you to keep the surface.

Claims (4)

Method for producing a water-repellent semi-coated zeolite consisting of the following steps: (1) dispersing 0.01-10 weight of methylhydrogen polysiloxane, 0.01-5 weight of cyclomethicone and 0.01-10 weight of active silane in an organic solvent; (2) adding 1-50 weight of the active zeolite to the reaction obtained in (1); And (3) warming to temperature 90-150 ° C. The method of claim 1, wherein the mixing ratio of the methylhydrogen polysiloxane and the cyclomethicone is 1: 4-4: 1. The method of claim 1, wherein the organic solvent is selected from the group consisting of isopropyl alcohol, anhydrous ethanol and anhydrous methanol. Non-aqueous exothermic cosmetics containing 0.5-60 weight of the semi-coated zeolite prepared by the method of claim 1.