Process for the production of an alcohol composition

Abstract

The present application aims to provide a method for producing an alcohol composition, which can adjust the viscosity to a suitable viscosity without using a process using heat treatment while using HPMC or MC as a thickening agent. The above object is solved by a method for producing an alcohol composition, which comprises: a process of obtaining a dispersion liquid by dispersing at least one water-soluble cellulose ether selected from the group consisting of hydroxypropyl methylcellulose and methylcellulose in a first alcohol; a process of obtaining a solution liquid by mixing the dispersion liquid and water and dissolving the water-soluble cellulose ether; and a process of obtaining an alcohol composition by mixing the solution liquid and a second alcohol.

Description

Technical Field

[0001] This invention relates to a method for manufacturing alcohol compositions. Background Technology

[0002] Alcohol compositions are widely used in industry and in households. For example, hand sanitizers containing monohydric alcohols and water, cold preservers for pharmaceuticals and food containing polyhydric alcohols, cosmetics such as hairspray, and fragrances are used in a variety of applications.

[0003] The demand for alcohol-based hand sanitizers has surged, particularly since 2020, with widespread use not only in medical and nursing settings but also in ordinary households. For example, high-viscosity gel-based hand sanitizers offer advantages such as being less likely to spill and being easy to carry. To manufacture gel-based hand sanitizers, viscosity adjustments are necessary.

[0004] As thickeners for adjusting the viscosity of alcohol compositions, acrylic polymers, polyvinyl alcohol, xanthan gum, cellulose derivatives, etc., can be used. For example, Patent Document 1 reports a method for obtaining an alcohol composition by using acrylic polymers, xanthan gum, and cellulose derivatives as thickeners (Patent Document 1).

[0005] In addition, a method was reported that hydroxypropyl methylcellulose (hereinafter also referred to as "HPMC") is used as a thickener in cellulose derivatives, and HPMC is added to a mixture of ethanol, phosphoric acid, trisodium phosphate, trisodium phosphate salt and glycerol and dispersed to obtain a suspension, and then purified water is added to obtain a disinfectant solution (Patent Document 2). Another method was reported that HPMC is dispersed in a heated mixture of alcohol and water and then dissolved by cooling for 4 hours to obtain an alcohol composition (Patent Document 3).

[0006] Existing technical documents

[0007] Patent documents

[0008] Patent Document 1: Japanese Patent Publication No. 2008-508189

[0009] Patent document 2 Japanese Patent Application Publication No. 2016-166134

[0010] Patent document 3 Japanese Patent Publication No. 2015-524425 Summary of the Invention

[0011] The problem that the invention aims to solve

[0012] According to the methods described in Patent Documents 1 to 3, alcohol compositions can be obtained. However, in the method described in Patent Document 1, there is a problem that the content of thickener in the alcohol composition is as low as 0.3%. Furthermore, in the method described in Patent Document 2, there is a problem that the solubility is insufficient, the viscosity is as low as 1,210 mPa·s, and it is difficult to adjust the viscosity. In the method described in Patent Document 3, since heating is required, there are time and cost issues due to the need for specialized manufacturing equipment and a cooling process after heating.

[0013] One of the reasons for the aforementioned problems is that HPMC is insoluble in alcohols. Furthermore, methylcellulose (hereinafter also referred to as "MC"), used as a thickener, is also insoluble in alcohols. That is, if the methods described in Patent Documents 1-3 are not used, when preparing an alcohol composition containing HPMC or MC and a specified concentration of alcohol, sufficient hydration does not occur during dissolution, resulting in reduced transparency. Furthermore, due to insufficient dissolution, a highly viscous alcohol composition cannot be obtained.

[0014] Furthermore, in recent years, there has been an increasing awareness in society of the effective use of sustainable resources with lower environmental impact. From an environmental perspective, there is a desire to use sustainable resource components, primarily water-soluble cellulose ethers such as HPMC and MC, and to reduce the substitution of synthetic polymers and the amount of synthetic polymers used. To this end, there is a need for a method for manufacturing alcohol compositions that can use HPMC and MC as thickeners while avoiding the problems caused by the methods described in Patent Documents 1-3.

[0015] Therefore, the object of the present invention is to provide a method for manufacturing an alcohol composition that, while using HPMC or MC as a thickener, allows for viscosity adjustment to achieve a suitable viscosity without including a heat treatment step.

[0016] Methods for solving problems

[0017] Through dedicated research aimed at achieving the aforementioned objectives, the inventors discovered that by sequentially performing the following steps: dispersing water-soluble cellulose ethers such as HPMC and MC in a first alcohol to obtain a dispersion; mixing the dispersion with water to obtain a solution of the water-soluble cellulose ether; and mixing the solution with a second alcohol to obtain an alcohol composition, an alcohol composition with various properties and contents of water-soluble cellulose ethers and appropriate viscosity can be obtained even without performing a heat treatment step. Furthermore, based on this insight, the inventors successfully developed a method for manufacturing an alcohol composition comprising the above-described steps. This invention is based on the insights and successful examples first discovered by the inventors.

[0018] Therefore, according to the present invention, a method for manufacturing an alcohol composition and a kit are provided in the following manner:

[0019] [1]. A method for manufacturing an alcohol composition, comprising: a step of dispersing at least one water-soluble cellulose ether selected from hydroxypropyl methylcellulose and methylcellulose in a first alcohol to obtain a dispersion;

[0020] The process of dissolving the water-soluble cellulose ether by mixing the dispersion with water to obtain a solution; and,

[0021] The process of obtaining an alcohol composition by mixing the solution and the second alcohol.

[0022] [2]. According to the method for manufacturing the alcohol composition described in [1], the ratio of the mass of the first alcohol to the total mass of the first alcohol and the second alcohol ([first alcohol] / [first alcohol + second alcohol]) is 0.70 or less.

[0023] [3]. According to the method of manufacturing alcohol composition described in [1] or [2], the first alcohol and / or the second alcohol is at least one alcohol selected from lower alcohols having 1 to 4 carbon atoms and polyols.

[0024] [4]. In the method of manufacturing the alcohol composition according to [1] or [2], the first alcohol and / or the second alcohol is at least one alcohol selected from ethanol, isopropanol and glycerol.

[0025] [5]. In the method of manufacturing the alcohol composition according to [1] or [2], the first alcohol and / or the second alcohol is ethanol, and the total content of the alcohol is 60.0% by mass to 90.0% by mass.

[0026] [6]. A kit for manufacturing alcohol compositions, comprising: at least one water-soluble cellulose ether selected from hydroxypropyl methylcellulose and methylcellulose;

[0027] First alcohols;

[0028] Second alcohols;

[0029] Furthermore, the ratio of the mass of the first alcohol to the total mass of the first alcohol and the second alcohol ([first alcohol] / [first alcohol + second alcohol]) is 0.70 or less.

[0030] Invention Effects

[0031] According to the present invention, an alcohol composition having a desired viscosity, exhibiting a suitable viscous gel-like consistency, can be obtained while using water-soluble cellulose ethers such as environmentally friendly hydroxypropyl methylcellulose and methylcellulose, even without undergoing a heat treatment process. Furthermore, since the alcohol composition obtained according to the present invention can have a high alcohol concentration, it is useful as a method for manufacturing a gel-like disinfectant alcohol composition. Detailed Implementation

[0032] The following describes in detail one method for manufacturing an alcohol composition according to the present invention (hereinafter referred to as the "method") and a kit for the alcohol composition (hereinafter referred to as the "kit"). However, the present invention can be carried out in various ways as long as its purpose is achieved.

[0033] Unless otherwise specified, all terms used in this specification are used in their common sense as understood by those skilled in the art and should not be unduly interpreted as having a limited meaning. Furthermore, any speculations or inferences made in this specification are based on the insights or experience of the inventors to date, and the invention is not limited to such speculations or inferences.

[0034] The term "composition" is not specifically limited in its commonly used meaning; for example, it can refer to a combination of two or more ingredients.

[0035] The term "and / or" refers to any one of the listed related items, or any combination of two or more, or all of the combinations.

[0036] "Content" and "dosage" are synonymous with "content," referring to the ratio of the amount of an ingredient to the total amount of the composition. In this specification, unless otherwise defined, the unit of content is "mass % (wt%)." However, the total content of an ingredient shall not exceed 100%.

[0037] The "~" in numerical range indicates a range that includes the values ​​before and after it. For example, "0% to 100%" refers to the range above 0% and below 100%. "Exceeding" and "insufficient" refer to the lower and upper limits, respectively, without including the values ​​before them. For example, "exceeding 1" means a value greater than 1, and "insufficient to 100" means a value less than 100.

[0038] "Including" means that elements other than the explicitly stated elements can be added to what is included (synonymous with "at least including"), including "composed of" and "essentially composed of". That is, "including" can mean including the explicitly stated elements as well as any one or more of the explicitly stated elements, being composed of the explicitly stated elements, or being substantially composed of the explicitly stated elements. Examples of elements include: ingredients, processes, conditions, parameters, and other limiting information.

[0039] The number of digits in an integer value is the same as the number of significant digits. For example, 1 has one significant digit, and 10 has two significant digits. Similarly, the number of digits below the decimal point in a decimal value is the same as the number of significant digits. For example, 0.1 has one significant digit, and 0.10 has two significant digits.

[0040] One aspect of the present invention includes a method comprising: a step of obtaining a dispersion by dispersing at least one water-soluble cellulose ether selected from hydroxypropyl methylcellulose and methylcellulose in a first alcohol (hereinafter also referred to as the "step of obtaining the dispersion"); a step of obtaining a solution by dissolving the water-soluble cellulose ether by mixing the dispersion with water (hereinafter also referred to as the "step of obtaining the solution"); and a step of obtaining an alcohol composition by mixing the solution with a second alcohol (hereinafter also referred to as the "step of obtaining the alcohol composition").

[0041] In this specification, "water-soluble cellulose ether" refers to HPMC, MC, or both.

[0042] An alcohol composition manufactured by one method of the present invention, comprising water-soluble cellulose ethers such as HPMC and MC, water, and alcohols, or even when composed of these components, can have a very wide range of viscosities. Depending on the composition and properties of such an alcohol composition, the method of one method of the present invention is useful as a method for manufacturing alcohol disinfectant compositions such as gel-like alcohol disinfectant compositions.

[0043] <Process for obtaining the dispersion>

[0044] In the process of obtaining the dispersion, the dispersion is obtained by dispersing hydroxypropyl methylcellulose, methylcellulose, or both in a first alcohol.

[0045] [First alcohol]

[0046] In one embodiment of the present invention, the alcohol is prepared in two stages, comprising a first alcohol and a second alcohol. The first alcohol and the second alcohol can be of the same type or of different types. The alcohol is not particularly limited as long as it is miscible with water; examples include lower alcohols having 1 to 4 carbon atoms and polyols.

[0047] Examples of lower alcohols having 1 to 4 carbon atoms include methanol, ethanol, n-propanol, isopropanol, n-butanol, and tert-butanol. Examples of polyols include ethylene glycol, propylene glycol, 1,3-propanediol, dipropylene glycol, 1,3-butanediol, glycerol, diglycerol, and pentanediol. Among these, ethanol and isopropanol are preferred from the viewpoint of imparting a disinfecting effect to the alcohol composition, while glycerol is preferred from the viewpoint of versatility and imparting a moisturizing effect to the alcohol composition.

[0048] Alcohols can be used alone or in combination of two or more, for example, lower alcohols with 1 to 4 carbon atoms and polyols can be mixed.

[0049] The content of alcohols (the total mass of the first alcohol and the second alcohol) can be appropriately set according to the intended use of the alcohol composition, as long as it is an amount that can be dissolved by the water-soluble cellulose ether used, and is not particularly limited. For example, when the alcohol is ethanol or isopropanol, from the viewpoint of the solubility of the water-soluble cellulose ether, it is preferably 30.0% to 95.0% by mass, more preferably 40.0% to 95.0% by mass, and from the viewpoint of the disinfection properties of the alcohol composition, it is more preferably 50.0% to 95.0% by mass, and even more preferably 60.0% to 90.0% by mass. When the alcohol is glycerol, diglycerol, or a mixture of glycerol and diglycerol, from the viewpoint of the solubility of the water-soluble cellulose ether and the moisturizing properties of the alcohol composition, it is preferably 20.0% to 70.0% by mass, more preferably 20.0% to 60.0% by mass, and even more preferably 20.0% to 50.0% by mass, from the viewpoint of the solubility of the water-soluble cellulose ether and the moisturizing properties of the alcohol composition.

[0050] The content of the first alcohol is not particularly limited. However, in one aspect of the invention, by maintaining a certain relationship between the mass of the first alcohol and the total mass of the first and second alcohols, the solubility stability of the water-soluble cellulose ether in the alcohol composition can be improved, allowing the water-soluble cellulose ether to hydrate well. To achieve this sufficient hydration of the water-soluble cellulose ether, preferably, the ratio of the mass of the first alcohol to the total mass of the first and second alcohols ([first alcohol] / [first alcohol + second alcohol]; hereinafter referred to as "first alcohol content") is 0.70 or less, more preferably 0.61 or less. When this ratio exceeds 0.70, the water ratio in the solution becomes smaller in the subsequent step of obtaining the solution, which may result in insufficient water content to aid in the dissolution of the water-soluble cellulose ether, leading to insufficient hydration. Consequently, the water-soluble cellulose ether may not dissolve sufficiently, failing to achieve the desired thickening properties of the obtained alcohol composition.

[0051] For example, when the mass of the first alcohol is 20.0% by mass, and the ratio of the mass of the first alcohol to the total mass of the first alcohol and the second alcohol, i.e., the content of the first alcohol is 0.267, the total mass of the alcohol is 75.0% by mass, and the mass of the second alcohol is 55.0% by mass.

[0052] One aspect of the present invention involves dispersing a water-soluble cellulose ether in the first alcohol by dividing an alcohol into a first alcohol and a second alcohol. This eliminates the need for hot water for dispersion, which is required to prepare an aqueous solution of the water-soluble cellulose ether in advance. Furthermore, it reduces the time and electricity costs associated with the heat treatment and the subsequent cooling process to below the dissolution temperature.

[0053] Hydroxypropyl methylcellulose (HPMC)

[0054] HPMC is a water-soluble cellulose ether formed by introducing methoxy and hydroxypropoxy groups into cellulose. HPMC does not have particularly limited physical properties such as the degree of substitution of the methoxy group, the molar number of hydroxypropoxy groups, viscosity, and molecular weight; these properties can be appropriately selected according to the desired characteristics, such as viscosity, imparted to the resulting alcohol composition. The method of obtaining HPMC is not particularly limited; it can be manufactured using methods known to date, or it can be obtained as a commercially available product.

[0055] As a method for manufacturing HPMC, water-soluble hydroxypropyl methylcellulose can be prepared by reacting an alkali in cellulose pulp to obtain alkali cellulose, then reacting the obtained alkali cellulose with a hydroxypropyl etherifying agent and a methylating agent, and then washing, drying, pulverizing, etc. on the obtained reactants.

[0056] The viscosity of HPMC is not particularly limited, but for example, in order to impart a desired viscosity to the alcohol composition, the viscosity of a 2.0% by mass aqueous solution of HPMC at 20°C is preferably 1,000 mPa·s to 120,000 mPa·s, more preferably 1,500 mPa·s to 100,000 mPa·s, and even more preferably 2,000 mPa·s to 100,000 mPa·s. When the viscosity of HPMC is 1,000 mPa·s to 120,000 mPa·s, regardless of the alcohol content obtained, the viscosity of the alcohol composition can have a viscosity that allows it to exhibit a desired form such as a gel or liquid. Furthermore, if the viscosity of a 2.0% by mass aqueous solution of HPMC at 20°C is less than 1,000 mPa·s, the thickening effect imparted to the alcohol composition is weak, and there is a possibility that the viscosity stability of the alcohol composition is insufficient. On the other hand, when the viscosity of a 2.0% by mass aqueous solution of HPMC at 20°C exceeds 120,000 mPa·s, the compatibility and solubility of HPMC and alcohols deteriorate, resulting in a possible decrease in the thickening and / or transparency of the alcohol composition. The viscosity of a 2.0% by mass aqueous solution of HPMC at 20°C was measured using a single-cylinder rotational viscometer according to the "Viscosity Measurement Method" of the General Test Method described in the 17th edition of the Japanese Pharmacopoeia, as described in the examples below.

[0057] From the viewpoints of alcohol dispersibility, alcohol compatibility, viscoelasticity of the alcohol composition, and transparency, the degree of methoxyl substitution (DS) in HPMC is preferably 1.00 or higher, more preferably 1.20 to 2.20, and even more preferably 1.3 to 2.1. The degree of methoxyl substitution (DS) refers to the average number of methoxy groups per unit of dehydrated glucose.

[0058] From the viewpoints of dispersibility and compatibility of alcohols, viscoelasticity of the alcohol composition, and transparency, the molar substitution number (MS) of hydroxypropoxy groups in HPMC is preferably 0.1 or more, more preferably 0.10 to 0.60, and even more preferably 0.13 to 0.40. The molar substitution number (MS) of hydroxypropoxy groups refers to the average number of moles of hydroxypropoxy groups per unit of dehydrated glucose.

[0059] The DS of methoxy and the MS of hydroxypropoxy in HPMC were obtained by converting the values ​​measured using the determination method related to hydroxypropyl methylcellulose (hydroxypropyl methylcellulose) in the 17th revised edition of the Japanese Pharmacopoeia.

[0060] The content of HPMC can be appropriately set according to the desired thickening properties imparted to the alcohol composition, and is not particularly limited. For example, it is preferably 0.05% to 4.0% by mass, more preferably 0.1% to 3.8% by mass, further preferably 0.2% to 3.5% by mass, and even more preferably 0.5% to 3.0% by mass in the total mass of the alcohol composition.

[0061] [Methylcellulose (MC)]

[0062] MC is a water-soluble cellulose ether formed by introducing methoxy groups into cellulose. The physical properties of MC, such as the degree of methoxy substitution, viscosity, and molecular weight, are not particularly limited, and can be appropriately selected according to the desired characteristics, such as viscosity, imparted to the resulting alcohol composition. The method of obtaining MC is not particularly limited; it can be manufactured using methods known to date, or it can be obtained as a commercially available product.

[0063] As a method for manufacturing MC, for example, water-soluble methylcellulose can be prepared by reacting an alkali in cellulose pulp to obtain alkali cellulose, then reacting the obtained alkali cellulose with a methylating agent, and then washing, drying, pulverizing, etc. on the obtained reactants.

[0064] The viscosity of MC is not particularly limited, but for example, in order to impart a desired viscosity to the alcohol composition, the viscosity of a 2.0% by mass aqueous solution of MC at 20°C is preferably 1,000 mPa·s to 50,000 mPa·s, more preferably 1,500 mPa·s to 40,000 mPa·s, and even more preferably 2,000 mPa·s to 30,000 mPa·s. When the viscosity of MC is 1,000 mPa·s to 50,000 mPa·s, regardless of the alcohol content obtained, the viscosity of the alcohol composition can have a viscosity that allows it to exhibit a desired form such as a gel or liquid. Furthermore, if the viscosity of a 2.0% by mass aqueous solution of MC at 20°C is less than 1,000 mPa·s, the thickening effect imparted to the alcohol composition is weak, and there is a possibility that the viscosity stability of the alcohol composition is insufficient. On the other hand, when the viscosity of a 2.0% by mass aqueous solution of MC at 20°C exceeds 50,000 mPa·s, the miscibility and solubility with alcohols decrease, resulting in a potential reduction in the thickening and / or transparency of the alcohol composition. The viscosity of the 2.0% by mass aqueous solution of MC at 20°C was measured using a single-cylinder rotational viscometer according to the viscosity determination method of the general test method described in the 17th edition of the Japanese Pharmacopoeia, as described in the examples below.

[0065] From the viewpoints of dispersibility and compatibility of alcohols, viscoelasticity of the alcohol composition, and transparency, the degree of substitution (DS) of methoxy groups in MC is preferably 1.00 to 2.20, more preferably 1.30 to 2.10, and even more preferably 1.50 to 2.00. The degree of substitution (DS) of methoxy groups refers to the average number of methoxy groups per unit of dehydrated glucose.

[0066] The content of MC can be appropriately set according to the desired thickening properties imparted to the alcohol composition, and is not particularly limited. For example, it is preferably 0.05% to 4.0% by mass, more preferably 0.1% to 3.5% by mass, further preferably 0.2% to 3.0% by mass, and even more preferably 0.5% to 2.2% by mass in the total mass of the alcohol composition.

[0067] The DS of the methoxy group in MC was calculated by converting the value determined using the determination method related to methylcellulose in the 17th revised edition of the Japanese Pharmacopoeia.

[0068] However, when using both HPMC and MC as water-soluble cellulose ethers, the total amount of water-soluble cellulose ethers can be appropriately set considering the aforementioned ranges for HPMC and MC, as well as their required thickening properties and solubility in alcohols.

[0069] [Process Conditions]

[0070] The conditions for dispersing water-soluble cellulose ethers in a first alcohol are not particularly limited, and conditions known to date for dispersing solids in a solvent can be used. For example, the water-soluble cellulose ether can be dispersed in a first alcohol by contacting the first alcohol and then mixing it with stirring or other methods, thereby obtaining a dispersion.

[0071] When mixing is used as a mixing process, the mixing method is not particularly limited, and the following mixing methods can be used: homogenizer, homogenizing mixer, homogenizing disperser, jet mixer, ultrasonic mixer, colloid mill, three-in-one motor, etc.

[0072] The stirring temperature is not particularly limited, but is preferably 0℃~40℃, and more preferably 0℃~35℃; the stirring time is not particularly limited, but is preferably 1 minute~30 minutes, and more preferably 5 minutes~15 minutes.

[0073] In the process of obtaining the dispersion, a homogeneous dispersion can be said to be obtained by visually confirming that there are no substantially no lumps (agglomerates (small powder particles)) of water-soluble cellulose ether, or that the water-soluble cellulose ether is in a state before mixing or is agglomerated. Furthermore, preferably, the dispersion remains homogeneous for at least one hour after standing. For good dispersion in the first alcohol, the water-soluble cellulose ether is preferably in powder form, and more preferably has an average particle size of 10 μm to 100 μm as determined by dry laser diffraction.

[0074] <Process for obtaining the solution>

[0075] In the process of obtaining the solution, the water-soluble cellulose ether is dissolved by mixing the dispersion obtained in the process of obtaining the dispersion with water.

[0076] [water]

[0077] Water is not particularly limited; examples include ion-exchanged water, distilled water, and tap water. Additionally, aqueous solutions containing salts, water-soluble polymers, etc., can also be used, as long as they can dissolve water-soluble cellulose ethers.

[0078] Although the water content can be appropriately set according to the amount of water-soluble cellulose ether, the higher the water content, the greater the amount of water-soluble cellulose ether dissolved. The water content only needs to be the amount necessary for the dissolution of the water-soluble cellulose ether or more. For example, when the alcohol is ethanol or isopropanol, the water content in the total mass of the alcohol composition is preferably 4.9% to 69.9% by mass, more preferably 4.9% to 59.9% by mass, even more preferably 4.9% to 49.9% by mass, and even more preferably 4.9% to 39.9% by mass. When the alcohol is glycerol, diglycerol, or a mixture of glycerol and diglycerol, the water content in the total mass of the alcohol composition is preferably 26% to 79.9% by mass, more preferably 36% to 79.9% by mass, and even more preferably 46% to 79.9% by mass.

[0079] The water temperature can be appropriately set according to the type of water-soluble cellulose ether, for example, 0℃~35℃. Considering the property that water-soluble cellulose ethers have higher solubility at lower temperatures, 0℃~30℃ is preferred, and 0℃~20℃ is even more preferred.

[0080] [Process Conditions]

[0081] The conditions under which the dispersion and water are mixed to dissolve the water-soluble cellulose ether are not particularly limited, and conditions known to date for dissolving substances in the dispersion in water can be used. For example, from an operational point of view, it is preferable to add water to the dispersion and mix it.

[0082] As a mixing process, stirring is preferred. The stirring method is not particularly limited, and examples include: homogenizers, homogenizing mixers, homogenizing dispersers, jet mixers, ultrasonic mixers, colloid mills, and three-in-one motors. The stirring method can be the same as that used in the process of obtaining the dispersion, or it can be a different stirring method.

[0083] The stirring temperature is not particularly limited as long as it is the temperature at which the water-soluble cellulose ether dissolves, but is preferably 0°C to 35°C, and more preferably 0°C to 25°C. The stirring time is not particularly limited as long as it is the time it takes for the water-soluble cellulose ether to dissolve completely, but is preferably 10 minutes to 60 minutes.

[0084] In the process of obtaining the solution, a solution can be said to be obtained when it is visually confirmed that there is no substantial separation or precipitation of water-soluble cellulose ethers. In order to improve the solubility of water-soluble cellulose ethers, part or all of the process can be carried out simultaneously with cooling in the process of obtaining the solution.

[0085] [Process for obtaining the alcohol composition]

[0086] In the process of obtaining the alcohol composition, the alcohol composition is obtained by mixing the solution obtained in the process of obtaining the solution with the second alcohol.

[0087] [Second alcohols]

[0088] As mentioned above, the second alcohol can be of the same type as the first alcohol or a different type. The content of the second alcohol is not particularly limited, but to achieve good hydration of the water-soluble cellulose ether in the alcohol composition, it is preferable that the ratio of the mass of the first alcohol to the total mass of the first alcohol and the second alcohol ([first alcohol] / [first alcohol + second alcohol]) is 0.70 or less.

[0089] [Process Conditions]

[0090] The conditions for mixing the solution and the second alcohol to obtain the alcohol composition are not particularly limited, and conditions for mixing liquids together, as known to date, can be used. For example, from an operational point of view, it is preferable to add the second alcohol to the solution and mix it by stirring or the like. The stirring means is not particularly limited, and examples of stirring devices such as homogenizers, homogenizing mixers, homogenizing dispersers, jet mixers, ultrasonic mixers, colloid mills, and three-in-one motors can be used. The stirring means can be the same as that used in the process of obtaining the dispersion and / or the process of obtaining the solution, or it can be a different stirring means. However, in order to improve the solubility stability of the water-soluble cellulose ether in the alcohol composition and the homogeneity of the components in the alcohol composition, it is preferable to subject the solution and the second alcohol to vigorous mixing, more preferably vigorous mixing, and even more preferably homogenization.

[0091] The stirring temperature is not particularly limited, but is preferably 0℃ to 35℃, and more preferably 0℃ to 25℃. The stirring time is not particularly limited, but is preferably 20 minutes to 90 minutes.

[0092] In the process of obtaining the alcohol composition, the alcohol composition can be said to be obtained when it is visually confirmed that there is substantially no separation or precipitation of water-soluble cellulose ethers. If the dissolution of water-soluble cellulose ethers is insufficient, the separated or precipitated portion of the water-soluble cellulose ethers tends to precipitate after the alcohol composition has been left to stand for one week. Therefore, the alcohol composition is preferably one in which, after standing for one week, no separation or precipitation of water-soluble cellulose ethers is visually observed to have occurred. In the process of obtaining the alcohol composition, in order to improve the solubility of water-soluble cellulose ethers, part or all of the process can be carried out simultaneously with cooling.

[0093] In one aspect of the present invention, various steps or operations can be added before or after the above-mentioned steps, or in the process itself, as long as the problem of the present invention can be solved. However, it is preferable that the process is carried out continuously without inserting other steps between the steps of obtaining the dispersion, obtaining the solution, and obtaining the alcohol composition.

[0094] <Alcohol Compositions>

[0095] The alcohol composition obtained according to one method of the present invention is not particularly limited in terms of its physical properties and uses, as long as it is obtained according to one method of the present invention. The alcohol composition manufactured according to one method of the present invention can have a viscosity set over a wide range. For example, the viscosity of the alcohol composition at 20°C can be set from 100 mPa·s to 50,000 mPa·s, and it can be obtained in gel, liquid, or other forms.

[0096] The alcohol composition manufactured according to one method of the present invention can reduce the loss tangent (tanδ) and / or increase the light transmittance. For example, from the viewpoint of providing a good spreadability, the alcohol composition can set the loss tangent (tanδ) to 0.05 to 5.00, and by further setting the loss tangent (tanδ) to 1.00 or less, liquid dripping can be suppressed, resulting in a gel-like form with excellent spreadability and less viscosity. For example, the alcohol composition can set the light transmittance to 10.0% to 99.0%, and by further setting the light transmittance to 65.0% or more, a form with high transparency and excellent appearance can be obtained.

[0097] Furthermore, one method of the present invention can produce an alcohol composition with a loss tangent (tanδ) of 1.00 or less and a light transmittance of 65.0% or more. This alcohol composition is useful as a gel-like alcohol composition that combines excellent viscoelasticity and high transparency.

[0098] Furthermore, by setting the content of the alcohol composition to 60.0% by mass or more, it is useful as a gel-form alcohol-based disinfectant composition that, in addition to excellent viscoelasticity and high transparency, also possesses disinfectant properties. Additionally, by using glycerin as the alcohol, it is useful as a gel-form alcohol-containing cosmetic composition that, in addition to excellent viscoelasticity and high transparency, also possesses moisturizing properties.

[0099] The viscosity, loss tangent (tanδ), and transmittance of the alcohol composition were obtained by the methods described in the examples below. The liquid dripping and spreadability of the alcohol composition were confirmed by the methods described in the examples below.

[0100] Furthermore, during their research, the inventors discovered that by setting the degree of substitution (DS) of the methoxy group of the water-soluble cellulose ether and the molar number of substitutions (MS) of the hydroxypropoxy group, the alcohol concentration (mass %, X), and the content of the first alcohol (%) in a certain relationship, it is possible to manufacture an alcohol composition with a desired viscosity, low loss tangent (tanδ), and / or high transmittance.

[0101] That is, by using the method of one aspect of the present invention described above, if DS, MS, X, and Y, and Z calculated based on these values ​​according to the following formula, are set to the relationships described in Tables 1 to 3 below, then alcohol compositions having desired viscosity and low loss tangent (tanδ) can be obtained (Table 1); alcohol compositions having desired viscosity and high transmittance (Table 2); and alcohol compositions having desired viscosity, low loss tangent (tanδ), and high transmittance (Table 3).

[0102] (DS+MS) / X×Y=Z (where X>Y)

[0103] In Tables 1-3, the water-soluble cellulose ether used in Condition I is MC, and the water-soluble cellulose ether used in Conditions II-IV is HPMC. Furthermore, the values ​​for DS, MS, X, Y, and Z in Tables 1-3 are guideline values ​​and should not be interpreted as requiring these values ​​to be within the range necessary to manufacture various alcohol compositions.

[0104] Table 1

[0105] condition DS MS X Y Z I 1.00～2.20 0.00 43.0～80.0 10～70 0.21～3.10 II 1.50～2.20 0.15～0.35 43.0～93.0 10～70 0.22～3.50 II 1.50～2.20 0.10～0.21 43.0～80.0 10～70 0.22～3.15 IV 1.00～1.80 0.10～0.30 43.0～80.0 10～70 0.20～2.85

[0106] Table 2

[0107] condition DS MS X Y Z I 1.00～2.20 0.00 30.0～68.0 10～70 0.25～2.40 II 1.50～2.20 0.15～0.35 30.0～88.0 10～70 0.23～2.60 II 1.50～2.20 0.10～0.21 30.0～75.0 10～70 0.22～2.30 IV 1.00～1.80 0.10～0.30 30.0～70.0 10～70 0.21～2.10

[0108] Table 3

[0109] condition DS MS X Y Z I 1.00～2.20 0.00 43.0～80.0 10～70 0.24～3.10 II 1.50～2.20 0.15～0.35 43.0～88.0 10～70 0.23～3.50 II 1.50～2.20 0.10～0.21 43.0～75.0 10～70 0.22～3.15 IV 1.00～1.80 0.10～0.30 43.0～70.0 10～70 0.21～2.85

[0110] In Tables 1-3, from the viewpoint of the solubility of HPMC in the alcohol composition and the thickening properties imparted to the alcohol composition, the DS and MS of the HPMC used in conditions II-IV are preferably in a specified relationship. For example, the HPMC used in condition II preferably has a DS of 1.60-2.10 and an MS of 0.17-0.30; the HPMC used in condition III preferably has a DS of 1.60-2.10 and an MS of 0.12-0.21; and the HPMC used in condition IV preferably has a DS of 1.20-1.70 and an MS of 0.17-0.30.

[0111] In one aspect of the present invention, in order to impart the desired properties to the alcohol composition, other additives may be used in addition to HPMC, MC, alcohols, and water.

[0112] Additives are not particularly limited as long as they do not hinder the solution of the problem of the present invention. Examples include bactericides, viscosity modifiers, pH modifiers, fragrances, pigments, dyes, antioxidants, preservatives, humectants, etc.

[0113] Examples of fungicides include benzalkonium chloride, triclosan, and cypress alcohol.

[0114] Examples of viscosity modifiers include water-soluble polymers such as guar gum, locust bean gum, carboxymethyl cellulose, hydroxyethyl cellulose, hydrophobic hydroxypropyl methyl cellulose, cationic hydroxyethyl cellulose, carboxyvinyl polymers, and polyvinyl alcohol.

[0115] Examples of pH adjusters include: alkali metal hydroxides such as sodium hydroxide and potassium hydroxide; alkaline earth metal hydroxides such as calcium hydroxide and magnesium hydroxide; ammonium carbonate; ammonia; ammonia water; trisodium phosphate; disodium hydrogen phosphate; dipotassium hydrogen phosphate; alkyl secondary amines such as dimethylamine and diethylamine; alkyl tertiary amines such as trimethylamine and triethylamine; monoethanolamine; isopropanolamine; diethanolamine; diisopropanolamine; triethanolamine; triisopropanolamine; polyethanolamine, etc.

[0116] Examples of fragrance ingredients include: rose oil, jasmine oil, lavender oil, ylang-ylang oil, peppermint oil, geranium oil, patchouli oil, sandalwood oil, cinnamon oil, lemon oil, orange oil, bergamot oil, limonene, β-caryophyllene, cis-3-hexenol, linalool, farnesol, β-phenylethanol, 2,6-nonadienol, citral, d-hexylcinnamaldehyde, 1-carvone, cyclopentadecanol, linalyl acetate, γ-undecyl lactone, nerolidin, etc.

[0117] Examples of pigments include: titanium dioxide, zinc oxide, barium sulfate, zinc oxide coated or compounded with silicic anhydride, iron oxide (Indian red), iron titanate, γ-iron oxide, yellow iron oxide, loess, black iron oxide, carbon black, and low-valent titanium oxide.

[0118] Examples of dyes include: acid dyes, nitro dyes, disperse dyes, basic dyes, and intermediates of oxidative dyes.

[0119] Examples of antioxidants include: tocopherol, tocopherol acetate, ascorbic acid, butylated hydroxyanisole, and butylated hydroxytoluene.

[0120] Examples of preservatives include methylparaben, ethylparaben, propylparaben, butylparaben, and phenoxyethanol.

[0121] Examples of moisturizers include: hyaluronic acid, sodium hyaluronate, polyethylene glycol, mucopolysaccharides, urea, sorbitol, chondroitin sulfate, pyrrolidone carboxylic acid, sodium lactate, and polyaspartic acid.

[0122] The additives can be used alone or in combination with two or more of the above-mentioned additives. Furthermore, both commercially available additives and additives manufactured using methods known to date can be used.

[0123] The content of the additive is appropriately varied depending on the desired properties imparted to the alcohol composition and its intended use. For example, from the viewpoint of the storage stability of the alcohol composition, it is preferably 0.001% to 20.0 parts by mass.

[0124] <Reagent Kit>

[0125] In another embodiment of the invention, a kit for manufacturing alcohol compositions is provided for carrying out one embodiment of the invention. The kit of one embodiment of the invention comprises: at least one water-soluble cellulose ether selected from hydroxypropyl methylcellulose and methylcellulose; a first alcohol; and a second alcohol. However, the mass ratio of the first alcohol to the total mass of the first alcohol and the second alcohol ([first alcohol] / [first alcohol + second alcohol]) is 0.70 or less, preferably 0.61 or less.

[0126] In addition to water-soluble cellulose ethers, a first alcohol, and a second alcohol, the kit of one embodiment of the present invention may also contain other ingredients. Examples of such other ingredients include, but are not limited to, water; bactericides, viscosity modifiers, pH adjusters, fragrances, pigments, dyes, antioxidants, preservatives, and humectants.

[0127] In one embodiment of the kit of the present invention, each component is preferably placed in a separate container; however, for example, the first alcohol and the second alcohol may be placed in the same container. When the first alcohol and the second alcohol are placed in the same container, it is preferable, for example, to indicate the amount of each alcohol in a manner such as by marking a line in the container containing the alcohols, so that the mass of the first alcohol and the mass of the second alcohol are in the aforementioned mass ratio.

[0128] For the kit of one aspect of the present invention, the containers containing the various components are not particularly limited, and examples include packaging containers made of materials such as metals like aluminum, paper, polyethylene terephthalate, plastics such as blister packs (PTP), and glass. Preferably, the kit of one aspect of the present invention includes an instruction manual or packaging that describes the method of one aspect of the present invention.

[0129] [Example]

[0130] The present invention will be further described in detail below through embodiments and comparative examples. However, the present invention is not limited to these embodiments or comparative examples.

[0131] <Physical Property Evaluation>

[0132] [HPMC and the viscosity of MC]

[0133] For the viscosity of water-soluble cellulose ethers of HPMC and MC, the viscosity of a 2.0% by mass aqueous solution at 20°C was determined using a single-cylinder rotational viscometer according to the "Viscosity Measurement Method" of the General Test Method described in the 17th revised edition of the Japanese Pharmacopoeia.

[0134] [Viscosity of alcohol compositions]

[0135] The viscosity of the alcohol composition was measured using a single-cylinder viscometer (Tokyo Keiki Co., Ltd., "DVM-BII", rotor No. 2-4), as the value measured after 120 seconds at 30°C at 20°C. For viscometers exceeding 20,000 mPa·s, a type B viscometer (Tokyo Keiki Co., Ltd., "B8H", rotor No. 5) was used, and the value measured after 120 seconds at 20°C at 20°C.

[0136] [Loss Tangent]

[0137] For alcohol compositions, the loss tangent was measured using a rheometer “MCR-301” (manufactured by Anton Paar) as follows.

[0138] The sample measuring section of the rheometer was preheated to 25°C. The alcohol composition was injected into the mark (25 ml) of a CC27 measuring cup (a cylindrical aluminum container with a diameter of 30 mm and a height of 80 mm). For the alcohol composition injected into the measuring cup, deformation was applied within the range of 0.01% to 100.0% using a pump cylinder (26.7 mm in diameter and 40.0 mm in height: CC27), and the viscoelasticity was measured. The measuring section was kept constant at 25°C. The measured viscoelastic value was taken as the loss tangent.

[0139] [Light transmittance]

[0140] For alcohol compositions with a temperature setting of 20°C, the transmittance was measured using a photoelectric colorimeter "PC-50" (manufactured by KOTAKI) through a 720nm filter and a 20mm cuvette.

[0141] [Liquid dripping]

[0142] Place the alcohol composition into a dispenser container (“200ml pump bottle”, 3mm diameter, FRCOLOR Corporation), and visually confirm the liquid-free properties when dispensed as a gel three times consecutively. Evaluate the liquid droplet according to the following evaluation criteria.

[0143] Evaluation Criteria:

[0144] - No liquid dripping

[0145] +: When pressed 3 times, liquid drips when pressed 1 time.

[0146] ++: When pressed 3 times, liquid drips when pressed 2 times.

[0147] +++: When pressed 3 times, liquid drips.

[0148] <Sensory Evaluation>

[0149] [Applying feel]

[0150] The application feel was confirmed by five reviewers specializing in evaluating the user experience of alcohol-based compositions, using sensory evaluation as follows.

[0151] That is, each reviewer placed 5 ml of the alcohol composition on the back of their hand and scored the overall feel of the application based on the following evaluation criterion-a. The score with the highest number of responses was then used as the application feel. However, for compositions with a loss tangent exceeding 1.0 and a transmittance exceeding 65.0%, since they do not have an effect on the application feel, other evaluation criteria were established (evaluation criterion-b).

[0152] Evaluation Criteria - a

[0153] 3: It stretches well, has no stickiness, and feels relatively dry.

[0154] 2: Spreads well and feels moist when applied.

[0155] 1: It has a sticky feeling

[0156] 0: Poor spreadability, or liquid overflows from the hands and is difficult to apply.

[0157] Evaluation Benchmark - b

[0158] 2: Does not spill from hands, can be applied and is less sticky.

[0159] 1. It does not spill from your hands; it can be applied topically.

[0160] 0: Liquid spills from hands and is difficult to apply.

[0161] <Method for manufacturing alcohol compositions>

[0162] [Materials Used]

[0163] HPMC and MC used the samples listed in Table 4 (all manufactured by Shin-Etsu Chemical Co., Ltd.). Alcohols used were ethanol (manufactured by Fujifilm and Koichi Chemical Co., Ltd.), isopropanol (manufactured by Kishida Chemical Co., Ltd.), and glycerol (manufactured by Kishida Chemical Co., Ltd.). Purified water was used.

[0164] Table 4

[0165]

[0166] [Example 1]

[0167] Accurately weigh 20.0 g of ethanol as the first alcohol in a 200 ml beaker, add 2.0 g of MC (CE-1), and stir for 2 minutes using a magnetic stirrer (Azov Corporation, "HS-360", 200 rpm to 300 rpm) to form a homogeneous dispersion. Then, while maintaining stirring, add 28.0 g of pure water at 20°C to the resulting dispersion to dissolve the MC and obtain a solution. Add 50.0 g of ethanol as the second alcohol to the resulting solution and homogenize for 4 minutes using a small homogenizer (Azov Corporation, "AHG-160D", 5,000 rpm) to obtain the alcohol composition of Example 1.

[0168] [Examples 2-24 and 26-39]

[0169] Except for the types and amounts of alcohols and samples shown in Table 5, the alcohol compositions of Examples 2-24 and 26-39 were prepared in the same manner as in Example 1.

[0170] [Example 25]

[0171] Carboxyvinyl polymer (2.0 g) was added to pure water (98.0 g) and dissolved using a homogenizer (Azovn HM-310) to prepare a 2% aqueous solution of carboxyvinyl polymer (carbomer).

[0172] Accurately weigh 20.0 g of ethanol into a 200 ml beaker, add 2.0 g of hydroxypropyl methylcellulose, and stir for 2 minutes using a magnetic stirrer (Azov Corporation, "HS-360", 200 rpm to 300 rpm) to form a homogeneous dispersion. Then, while maintaining stirring, add 17.8 g of pure water at 20°C and 10.0 g of a 2.0% by mass aqueous solution of carbomer to dissolve HPMC. Add 50.0 g of ethanol to the resulting solution, homogenize at 5,000 rpm for 4 minutes using a small homogenizer (Azov Corporation, "AHG-160D"), and then add triethanolamine to adjust the pH to 6 to 8 to obtain the alcohol composition.

[0173] [Example 40]

[0174] Accurately weigh 20.0 g of ethanol into a 200 ml beaker, add 2.0 g of hydroxypropyl methylcellulose (HPMC), and stir for 2 minutes using a magnetic stirrer (Azov, HS-360, 200-300 rpm) to form a homogeneous dispersion. Then, while maintaining stirring, add 26.0 g of pure water at 20°C to the dispersion to dissolve the HPMC. Add 50.0 g of ethanol and 2.0 g of glycerol to the resulting solution, and homogenize at 5,000 rpm for 4 minutes using a small homogenizer (Azov, AHG-160D) to obtain the alcohol composition.

[0175] [Comparative Examples 1-3]

[0176] Except for the types and amounts of alcohols and samples shown in Table 5, the alcohol compositions of Comparative Examples 1 to 3 were prepared in the same manner as in Example 1. However, the second alcohol was not used when preparing the alcohol compositions of Comparative Examples 1 to 2, and the first alcohol was not used when preparing the alcohol composition of Comparative Example 3.

[0177] <Evaluation Results>

[0178] The results of evaluating viscosity, loss tangent, transmittance, liquid dripping, and spreadability for the alcohol compositions of Examples 1-40 are shown in Tables 5 and 6.

[0179] In the methods for manufacturing the alcohol compositions of Examples 1-40, since hot water is not used, a hot water cooling step is unnecessary, reducing time and electricity consumption. Furthermore, since an aqueous solution of HPMC or MC is not prepared beforehand, the alcohol compositions can be prepared in a one-pot process.

[0180] The alcohol compositions of Examples 1-40 can use various alcohols, HPMC or MC can be well dissolved, and the viscosity can be adjusted in a wide range from 629 mPa·s to 25,250 mPa·s.

[0181] In contrast, in the alcohol compositions of Comparative Examples 1 and 2, HPMC did not dissolve, and after standing for a week, the precipitated HPMC formed. When preparing the alcohol composition of Comparative Example 3, when HPMC powder was added to water, the surface of the powder clumps dissolved first, and the water did not penetrate the interior of the clumps, resulting in small clumps (agglomerates). The alcohol compositions of Comparative Examples 1-3 not only had a poorer appearance, but also, because the HPMC did not dissolve, did not achieve a sufficient thickening effect, making viscosity measurement impossible.

[0182] In the alcohol compositions of Examples 1-40, those with a loss tangent of 1.00 or less maintained a good gel form because the contribution of elasticity outweighed the contribution of viscosity. As a result, no liquid dripped from the container, and it did not spill from the hand even when held in the hand, thus allowing for easy application. Furthermore, those with a loss tangent of 1.00 or less generally spread well, were easy to apply, had little stickiness, and provided a good user experience.

[0183] The alcohol compositions in Examples 1-40 with a light transmittance of 65.0% or more exhibit high transparency and a good appearance. Furthermore, those with a light transmittance of 65.0% or more and a loss tangent exceeding 1.00 have a weaker gel-like feel and a slippery liquid consistency, allowing for application without spilling from hands.

[0184] The alcohol compositions of Examples 1-40 with a loss tangent of 1.00 or less and a transmittance of 65.0% or more can maintain a good gel morphology, without liquid dripping, with high transparency and good appearance, and also have an excellent user experience.

[0185] The alcohol compositions in Examples 1-40, which contain glycerin as an alcohol, not only have good properties but also a moisturizing feel, resulting in an excellent user experience.

[0186] Furthermore, the alcohol compositions of Examples 1-40, in common, exhibited a viscosity that remained almost unchanged after preparation, even after standing at room temperature for a week, due to the thorough dissolution of the water-soluble cellulose ethers they contained. Therefore, it can be concluded that although water-soluble cellulose ethers are poorly soluble in alcohols, they dissolve well in alcohol compositions.

[0187] Table 5

[0188]

[0189]

[0190]

[0191] Table 6

[0192]

[0193] Industrial availability

[0194] The method for manufacturing an alcohol composition according to one aspect of the present invention can be used in the medical field, personal care field, cosmetic field, etc., and can industrially manufacture alcohol compositions with desired viscosity and alcohol concentration.

Claims

1. A method for manufacturing an alcohol composition, comprising: a step of dispersing at least one water-soluble cellulose ether selected from hydroxypropyl methylcellulose and methylcellulose in a first alcohol to obtain a dispersion; The process of obtaining a solution by mixing the dispersion with water and dissolving the water-soluble cellulose ether; and, The process of obtaining an alcohol composition by mixing the solution and the second alcohol; The ratio of the mass of the first alcohol to the total mass of the first alcohol and the second alcohol is 0.70 or less; The first alcohol is at least one alcohol selected from lower alcohols having 1 to 4 carbon atoms and polyols; The second alcohol is at least one alcohol selected from lower alcohols having 1 to 4 carbon atoms and polyols.

2. The method for manufacturing the alcohol composition according to claim 1, wherein the first alcohol and / or the second alcohol is at least one alcohol selected from ethanol, isopropanol and glycerol.

3. The method for manufacturing the alcohol composition according to claim 1, wherein the first alcohol and / or the second alcohol is ethanol, and the total content of the first alcohol and the second alcohol is 60.0% by mass to 90.0% by mass.

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