JP2000302875A - Preparation of alcohol solution composition containing polymer compound and surfactant - Google Patents

Abstract

PROBLEM TO BE SOLVED: To prepare a transparent composition wherein the whitening or clouding generated by the addition of a polymer compound is inhibited, and to achieve an identical physical property among the compositions obtained from different batches when repetitively using the same blending tank without washing in a batch preparation of an alcohol solution composition containing a polymer compound and a surfactant. SOLUTION: In a process for preparing a transparent alcohol solution composition from a surfactant and a polymer compound which generates whitening or clouding when dissolved in an alcohol solution containing this surfactant, a portion of the alcohol is first mixed with the polymer compound and subsequently mixed with the rgmaining portion of the alcohol and the surfactant.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an alcohol solution composition containing a polymer compound and a surfactant, and more particularly, to a polymer compound capable of preventing cloudiness and turbidity caused by blending of the polymer compound. And a method for producing an alcohol solution composition containing a surfactant.

[0002]

2. Description of the Related Art
For example, in the case of blending a nonionic surfactant and a water-soluble polymer compound in various preparations, in an aqueous preparation using water as a solvent, the order of addition does not matter, but in an alcohol solution composition such as an ethanol preparation. Is added directly to the water-soluble polymer compound in ethanol in the mixing tank, and the water-soluble polymer compound is mixed with ethanol,
After swelling and dissolving, a method has been employed in which a nonionic surfactant is further added and mixed until the whole becomes uniform.

However, in this method, when the same blending tank is repeatedly used in a batch system and the next batch is manufactured without washing the blending tank, the second batch and the subsequent batches may be dissolved in water due to the effect of residual liquid. In addition, the system becomes cloudy at the time of addition of the hydrophilic polymer compound, and further, the viscosity is further lowered, so that there is a problem that a composition having the same physical properties as the first batch cannot be obtained.

[0004] The present invention has been made in view of the above circumstances, and is intended to prevent cloudiness and turbidity due to the addition of a polymer compound.
Provided is a method for producing an alcohol solution composition containing a polymer compound and a surfactant, which can produce a composition having the same physical properties every time even if the same compounding tank is used repeatedly without washing in a batch system. Aim to be.

[0005]

Means for Solving the Problems and Embodiments of the Invention The present inventors have conducted intensive studies in order to achieve the above object, and as a result,
The problem of white turbidity in continuous batch production has led to a focus on alcohol solution compositions of a specific composition, and as a result of further intensive studies on such alcohol solution compositions of a specific composition, the cause of white turbidity and turbidity But,
The interaction between the specific polymer compound and the surfactant in the composition, and the cloudiness occurs in the second and subsequent batches in the conventional method, is that the surfactant is contained in the remaining liquid in the blending tank. Is contained, this trace amount of surfactant swells in alcohol, and is found to be in contact with the polymer compound before dissolving in the alcohol. If it is allowed to swell or dissolve in part, and then comes into contact with a surfactant, a viscosity and a stable preparation in appearance can be obtained.For example, the polymer compound swells and dissolves in part of alcohol. If this polymer compound is mixed and dissolved in the rest of the alcohol in the blending tank, even if the surfactant is contained in the remaining liquid in the blending tank in the second and subsequent batches, The inventive polymer was found that can be dissolved in the remainder of the alcohol unaffected, leading to the completion of the present invention.

That is, the present invention relates to a method for producing a transparent alcohol solution composition from a surfactant and a polymer compound having a property of causing cloudiness or turbidity when dissolved in an alcohol solution containing the surfactant. An alcohol solution containing a polymer compound and a surfactant, wherein after mixing a part of the alcohol and the polymer compound, the mixture is mixed with the remainder of the alcohol and the surfactant. A method of making the composition is provided.

Hereinafter, the present invention will be described in more detail. The production method of the present invention comprises a surfactant, a polymer compound having a property of causing cloudiness when dissolved in an alcohol solution containing the surfactant, It mixes with alcohol.

Here, in the case of the present invention, the type of the alcohol is not particularly limited, and examples thereof include lower alcohols having 1 to 4 carbon atoms such as methanol, ethanol, isopropanol and butanol.
These can be used alone or in combination of two or more. In the case of the present invention, among them, ethanol is particularly preferable.

When the above alcohol is blended in the production method of the present invention, the alcohol may be 100% alcohol or a hydrated alcohol having an appropriate concentration. Here, when a water-containing alcohol is blended, the water content is preferably selected in consideration of a suitable water content in the whole composition described later.

In the present invention, the blending amount of the alcohol is not particularly limited, but is 60 to 97% (% by weight, hereinafter the same), particularly 80 to 95% with respect to the whole composition.
Is preferred. If the amount of the alcohol is too small, the viscosity increases, and the feeling of use and usability may decrease.If the amount is too large, a viscous solution that is one of the purposes of compounding the polymer compound into the composition is obtained. May not be. And, in the production method of the present invention, the mixing ratio of the alcohol, which is divided and divided into the first step and the second step as described below,
Although not particularly limited, the first step: the second step =
1: 0.5 to 1: 3, particularly preferably 1: 1 to 1: 1.5. Further, as described below, it is preferable that the weight concentration of the following polymer compound in the mixture obtained in the first step is 0.1 to 5%, particularly 0.5 to 2%.

The surfactant used in the present invention may be any surfactant having a property of making the solution cloudy when it comes into contact with the specific polymer compound in the alcohol solution. ,In particular,
For example, nonionic surfactants such as sucrose fatty acid esters, sorbitan fatty acid esters such as coconut oil sorbitan, and sorbitan monostearate; betaine acetate types such as lauryl dimethylaminoacetic acid betaine; Amphoteric surfactants such as amphoteric surfactants can be mentioned,
These can be used alone or in combination of two or more.

The amount of the above surfactant in the composition of the present invention is not particularly limited, but is 0.5 to 5%, preferably 1.5 to 2.5%, based on the whole composition. It is suitable. If the amount is too small, the effect of adding the surfactant may not be sufficiently obtained, and if the amount is too large, it may be difficult to prevent cloudiness.

Examples of the high molecular compound which becomes cloudy when it is mixed with the alcohol solution containing the surfactant include cellulose derivatives such as hydroxyethylcellulose, methylhydroxypropylcellulose, hydroxypropylcellulose and methylcellulose, and sugar-based polymers such as xanthan gum and guar gum. And a water-soluble polymer compound such as an alginic acid type such as propylene glycol alginate and a vinyl polymer such as a carboxyvinyl polymer. These can be used alone or in an appropriate combination of two or more. In the case of the present invention, among these, hydroxypropyl cellulose, carboxyvinyl polymer and the like are particularly preferred.

The amount of the above polymer compound in the composition of the present invention is not particularly limited, but is preferably 0.1 to 10%, more preferably 0.5 to 3%, based on the whole composition. is there. If the amount is too small, the effect of compounding the polymer compound may not be sufficiently obtained.

In the case of the present invention, the combination of the above-mentioned surfactant and a high molecular compound is a high molecular compound having the property of causing cloudiness or turbidity when dissolved in an alcohol solution containing the above surfactant. The combination thereof is not particularly limited, but examples of the surfactant include sucrose fatty acid esters, sorbitan fatty acid esters such as coconut fatty acid sorbitan and sorbitan monostearate, betaine lauryl dimethylaminoacetate, and coconut fatty acid. When a betaine acetate-type amphoteric surfactant such as amidopropyldimethylaminoacetic acid betaine is used, a carboxyvinyl polymer or the like is effective as the polymer compound.

In the production method of the present invention, as long as the effects of the present invention are not impaired, components other than the above-mentioned essential components can be blended. Specific examples of such components include fragrances, oils and fats,
Examples thereof include polyhydric alcohols, vitamins, hormones, and the like, which can be added in an appropriate amount. The water content of the composition obtained by the production method of the present invention is not particularly limited, but is preferably 0%.
-15%, more preferably 0-5%, particularly preferably 0-5%
１1% is preferred. If the water content is too high, a transparent composition can be obtained without using the production method of the present invention, and the effect of the present invention may be lost.

The production method of the present invention comprises a first step of mixing a part of the alcohol with the polymer compound, and a step of mixing the mixture obtained in the first step with the remainder of the alcohol and the surfactant. And a second step. Here, the stirrer used in these steps is not particularly limited, and for example, a simple mixing tank having a disperser or the like in the first step and a stirring tank having a paddle mixer in the second step. Can be used.

In the first step of the present invention, first, a part of the above alcohol and the above high molecular compound are charged into mixing tanks to prepare a mixture.
The polymer compound is added to the alcohol. Here, in the case of the present invention, the polymer compound is uniformly swelled or dissolved in a part of the alcohol in the first step, and the polymer compound is not sufficiently swollen or dissolved in the step. However, no matter how much time is spent in the subsequent steps, the system cannot be made turbid or cloudy. Further, the alcohol to be blended may contain an appropriate concentration of water as described above, and may further contain the above-mentioned optional components other than the above-mentioned surfactant. On the other hand, the above-mentioned polymer compound may be blended with any of the above-mentioned components as long as it is other than the above-mentioned surfactant, and may be further swollen in a solvent before mixing with a part of the alcohol. It may be placed or dispersed. In the case of the production method of the present invention, if the first step uses a mixing tank different from the mixing tank that performs the entire mixing in the second step, it is suitable for the case of manufacturing by a continuous batch method. .

When a part of the alcohol is mixed with the high molecular compound, the temperature is not particularly limited. For example, the temperature may be raised to 40 to 50 ° C. if necessary. The stirring conditions are not particularly limited. For example, the polymer compounds are mixed under ordinary stirring conditions such as a disperser until the polymer compound is uniformly swollen or dissolved.

In the second step of the present invention, a transparent alcohol solution containing the polymer compound and the surfactant is prepared by mixing the mixture with the remainder of the alcohol and the surfactant and other components. To obtain a composition. Here, the order of addition is not particularly limited, and the mixture, the remainder of the alcohol, and the surfactant are mixed with the optional components in advance before mixing them as necessary. Alternatively, a part thereof may be mixed in advance with each other.For example, the surfactant is previously dissolved in a part of the remaining portion of the alcohol in advance, and this is mixed in a mixing tank for performing the entire mixing. If you add
The mixing time after mixing the surfactant can be reduced.

In the case of the production method of the present invention, since the surfactant is not affected in the first and subsequent steps, the second and subsequent batches are used without washing the mixing tank in the continuous batch production method. Even if there is a residual liquid in the tank, the residual liquid containing the surfactant may be mixed with the remaining alcohol, for example, and the residual liquid containing the surfactant and the mixture may be mixed. And may be mixed. However,
In consideration of workability during continuous batch production, the remaining portion of the alcohol is put into a mixing tank for performing the entire mixing, and the mixture is added, mixed, and dissolved, and then the surfactant is further added. It is desirable to add and mix.

In the case of the second step, the temperature is not particularly limited. For example, the temperature can be raised to 30 to 50 ° C. if necessary. In addition, the stirring conditions are not particularly limited. For example, the mixture is uniformly mixed under the ordinary stirring conditions of a paddle mixer until a transparent solution is obtained.

In the production method of the present invention, an unneutralized (acid type) polymer compound such as a carboxyvinyl polymer is used as the polymer compound, and 2-amino-2-acid is used in the composition. When an alkaline component such as methyl-1-propanol is blended, the unneutralized polymer compound has a property of further increasing the viscosity when neutralized by the alkaline component in an alcohol solution. When the above-mentioned alkaline component is directly added to the alcohol solution of the molecular compound, the high-concentration alkaline component comes into contact with the high-molecular compound in the alcohol solution, and local gelation occurs at the portion where the alkaline component of the alcohol solution is added. Is generated to form a high-viscosity mass, and it may take a long time to homogenize the system. Therefore, in the case of such a composition, the alkaline component is dissolved in the alcohol, and the alkaline component is diluted, and then mixed with a mixture in which the polymer compound is swollen or dissolved in the alcohol. desirable.

The above-mentioned alcohol solution composition obtained by the production method of the present invention may be blended with the above-mentioned optional components, if necessary, to prepare hair cosmetics such as hair preparations, hair sprays and gels, body lotions, face lotions and the like. It can be used as various products such as a skin external preparation.

[0025]

According to the production method of the present invention, it is possible to produce a transparent composition while preventing cloudiness or turbidity due to the addition of the above-mentioned polymer compound. Therefore, the production method of the present invention provides an alcohol solution composition containing the above-mentioned polymer compound and the above-mentioned surfactant, for example, hair cosmetics such as hair restorer, hair spray and gel, and external skin preparations such as body lotion and face lotion. When manufacturing a product, a composition having the same physical properties can be produced every time even if it is used without washing the same mixing tank repeatedly in a batch system, and the polymer compound can be stably and easily prepared. It can be incorporated into the composition.

[0026]

EXAMPLES The present invention will be described in detail below with reference to examples and comparative examples, but the present invention is not limited to the following examples.

First, the following experiment was conducted in order to investigate the cause of white turbidity produced during the production. [Experimental Examples 1 to 3] Each of the hair restorers (alcohol solution compositions) shown in Table 1 was charged with ethanol into a blending tank and stirred in a 2 liter mixing tank at 1200 rpm using a paddle mixer. The raw materials were put into the mixing tank according to the order of addition in Table 1, and the solubility of each raw material and the appearance of the solution were visually observed and evaluated according to the following evaluation criteria. The results are also shown in Table 1. In the composition shown in Table 1, sucrose fatty acid esters (nonionic surfactants) were sucrose myristic acid ester (trade name: Ryoto Sugar Ester MWA-1695, manufactured by Mitsubishi Chemical Foods) and sucrose laurate ester (Product name: Ryoto Sugar Ester L
-595, manufactured by Mitsubishi Chemical Foods Corporation) at a polymerization ratio of 1: 3.

<Evaluation Criteria> Solubility ×: Mixing for 60 minutes after charging of the final component, scum was confirmed. Δ: When the final component was charged, a lump-like mass having high viscosity was formed locally.そ の 後: After mixing for 30 minutes, the mixture became uniform. ：: After mixing for 10 minutes after addition of the final component, the appearance was transparent without dissolving uniformly without discoloration . X: A little cloudiness was observed even after mixing for 60 minutes after charging the final component. Δ: When the final component was charged, it was slightly opaque due to the formation of lump-shaped lumps, but became transparent when mixed for 30 minutes thereafter. ○: Transparent when mixed for 10 minutes after charging the final component.

[0029]

[Table 1]

According to the results shown in Table 1, an ethanol solution composition (hair restorer) containing the sucrose fatty acid ester and a carboxyvinyl polymer which becomes cloudy when mixed with the ethanol solution of the sucrose fatty acid ester is produced. In this case, when sucrose fatty acid esters are dissolved in ethanol, and then a carboxyvinyl polymer is added thereto and mixed (Experimental Example 1), it is recognized that the system becomes cloudy and further crushing occurs.

On the other hand, when a carboxyvinyl polymer is dissolved in ethanol and then sucrose fatty acid esters are added and mixed (Experimental Examples 2 and 3), a transparent composition without crushing is finally obtained. However, when the high molecular compound used as the above hair restorer is a carboxyvinyl polymer which is an unneutralized high molecular compound, and 2-amino-2-methyl-1-propanol which is an alkaline component is further blended, When 2-amino-2-methyl-1-propanol is dissolved in ethanol and then mixed with a carboxyvinyl polymer (Experimental Example 3), a clear composition without crush can be easily produced. After dissolving the polymer in ethanol, undiluted 2-
When amino-2-methyl-1-propanol is added as it is (Experimental Example 2), it is recognized that it takes time to obtain a transparent composition without crush.

Example 1 and Comparative Example 1 According to the following composition, 47.8 of the total amount of ethanol (99.5 vol / vol% or more) was placed in a 2 liter mixing tank equipped with a paddle mixer.
% (Remainder), and 12% using the above paddle mixer.
While stirring the whole at 00 rpm, 2-amino-2-methyl-1-propanol was added, mixed and dissolved. Next, in another stirring tank equipped with a disper, 43.5% (part) of the total amount of ethanol in which a carboxyvinyl polymer (Carbopol 1342) was previously taken was added, and the mixture was stirred for 15 minutes with a disper to swell. Thus, a carbopol accessory (mixture) was prepared. The small carbopol was added to the mixing tank, and the mixture was stirred at 1200 rpm for 10 minutes using the paddle mixer until the whole was uniformly dissolved. Further, the same small sucrose fatty acid ester as in the above experimental example was previously dissolved in 8.7% of the total amount of ethanol, and the mixture was stirred at 1200 rpm using the paddle mixer until the whole was uniformly dissolved. After stirring for 15 minutes, an alcohol solution composition of Example 1 (intermediate product of a hair tonic) having the following composition was obtained, and after visually observing the appearance of the composition without residual liquid, the solution in the mixing tank was temporarily removed. The same process as above was performed by discarding and using the mixing tank without washing, and the appearance of the solution with residual liquid was visually observed.

On the other hand, in Example 1 above, the amount for pre-dissolving the sucrose fatty acid esters (8.
7%), except that ethanol (91.3% of the total amount) was charged into the blending tank, and the carboxyvinyl polymer was added as it was without making the carbopol accessory.
An alcohol solution composition of Comparative Example 1 (an intermediate product of a hair restorer) was obtained in the same manner as in Example 1 above, and after visually observing the appearance of the composition without residual liquid, the solution in the blending tank was once discarded. The same steps as above were performed using the mixing tank without washing, and the appearance of the solution with residual liquid was visually observed.

Composition Sucrose fatty acid esters 2.0% by weight Carboxyvinyl polymer 0.6 2-Amino-2-methyl-1-propanol 0.025 Ethanol Balance total 100.0

As a result of observing the difference between the production methods of Example 1 and Comparative Example 1, when there was no residual liquid in the blending tank, a transparent composition which was not opaque was obtained in all cases. When the tank was used, in the case of Comparative Example 1 in which the carboxyvinyl polymer was directly mixed with ethanol in the blending tank, the composition became a slightly cloudy composition, and the carboxyvinyl polymer was not swollen in advance in part of the ethanol. It was recognized that turbidity was caused by trace amounts of sucrose fatty acid esters and carboxyvinyl polymer contained in ethanol in the mixing tank. In the above observation, the amount of the residual liquid when there was a residual liquid was 0.5% of the total amount of the composition produced per batch, but thereafter, the observation was performed by changing the amount of the residual liquid. However, it was recognized that the cloudiness became clear as the amount of the residual liquid increased.

Example 2 After heating 47.8% (remainder) of the total amount of ethanol (99.5 vol / vol% or more) to 40 ° C. in a 2 liter mixing tank equipped with a paddle mixer, Pentadecanoic acid glyceride, tocopherol acetate,
l-Menthol and 2-amino-2-methyl-1-propanol were added and mixed and dissolved using the paddle mixer to prepare an ethanol solution. Next, in another stirring tank, carboxyvinyl polymer (Carbopol 1342) dispersed in ethyl oleate was added to 43.5% (part) of the total amount of ethanol taken in advance, and the mixture was stirred with a disper for 15 minutes. The mixture was swelled to prepare a small carbopol (mixture) having a compounding weight ratio of 92.81% of ethanol, 5.80% of ethyl oleate, and 1.39% of carboxyvinyl polymer. The Carbopol accessories were added to the ethanol solution and stirred at 1200 rpm for 10 minutes using the paddle mixer until the whole was uniformly dissolved. Further, the same small sucrose fatty acid ester in which the same sucrose fatty acid ester as in the above experimental example was previously dissolved was added to 8.7% of the total amount of ethanol, and the whole was uniformly dissolved using the paddle mixer. Up to 1200 rp
After stirring for 15 minutes at m, an alcohol solution composition (hair restorer) of Example 2 having the following composition was obtained. In addition, pentadecanoic acid glyceride is a nonionic surfactant, but does not affect cloudiness of the carboxyvinyl polymer.

Composition glyceride pentadecanoate 2.5% by weight Tocopherol acetate 0.2 Ethyl oleate 2.5 Sucrose fatty acid esters 2.0 1-Menthol 0.3 Carboxyvinyl polymer 0.6 2-Amino-2- Methyl-1-propanol 0.025 Ethanol Balance 100.0

According to the above-mentioned production method, five batches were continuously produced without washing the blending tank, and the resulting compositions were visually observed. No turbidity was observed in any of the batches. A composition having the same viscosity (about 920 cP) was obtained each time from the first batch to the fifth batch. In this example, the amount of residual liquid in the previous batch of the second and subsequent batches was about 5% by weight of the total amount of the composition produced per batch.

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Mototaka Kinoshita 1-3-7 Honjo, Sumida-ku, Tokyo Inside Lion Corporation (72) Inventor Masahiro Sato 1-3-7, Honjo, Sumida-ku, Tokyo No. Lion Corporation F term (reference) 4C083 AC101 AC102 AC422 AC542 AD011 AD092 AD222 AD532 AD662 BB01 CC37 DD23 EE22 4F070 AA01 AA02 AA28 AC36 AC43 AC45 AC72 AC94 AE14 CA02 CB02 4J002 AB011 AB031 AB051 AB052 AE052 AE052 AE052 HA05

Claims (1)

[Claims] When producing a transparent alcohol solution composition from a surfactant and a polymer compound having the property of causing cloudiness and turbidity when dissolved in an alcohol solution containing the surfactant, the alcohol is used to prepare a transparent alcohol solution composition. Preparation of an alcohol solution composition containing a polymer compound and a surfactant, characterized in that a part of the mixture is mixed with the polymer compound, and then the mixture is mixed with the remainder of the alcohol and the surfactant. Method.