JPH06319973A - Preparation of surfactant - Google Patents

Abstract

PURPOSE:To provide a method for preparation of a surfactant wherein impurities which causes change of smell for the worse, deterioration of hue and irritation can be extracted and eliminated efficiently by using an extractant (an extracting solvent) and an inexpensive apparatus and a surfactant with a high quality can be obtd. CONSTITUTION:The title method has a purification process wherein a water soln. of a surfactant contg. a component to be extracted is fed from a tower head part 5A of an extracting apparatus having a cylindrical extracting tower 1A and a plurality of perforated plates 2A arranged horizontally and in the longitudinal direction in the extracting tower 1A and an extractant for extracting a component to be extracted is fed from the tower bottom part 6A and extraction of the component to be extracted is performed while the interfacial position between the water soln. of the surfactant and the extractant is controlled so as to be kept it below the middle stage perforated plate 2A among the plurality of perforated plates 2A.

Description

Detailed Description of the Invention

[0001]

The present invention relates to an odor component, a coloring substance,
The present invention relates to a method for producing a surfactant from which impurities such as irritants have been removed, and particularly to a method for producing a surfactant suitable for the case where an extremely high purity such as a body wash is required.

[0002]

BACKGROUND OF THE INVENTION Surfactants are generally used in a variety of household products, industrial products, etc. as personal cleansers, industrial cleaners, food emulsifiers, softeners, antistatic agents, etc. Widely used in the field. Usually, when synthesizing the above-mentioned surfactant industrially, impurities such as reaction by-products and unreacted substances are contained in the product, and the odor of the surfactant is deteriorated due to these impurities. In many cases, the quality is deteriorated due to deterioration of hue, irritation and the like. In particular, when the surfactant is used as a personal cleanser or the like which is directly used or brought into contact with the human body, the presence of the above-mentioned impurities lowers the commercial value, and therefore the removal of these impurities is a very important matter.

For example, alkyl glycosides, which are sugar derivative surfactants, are suitable for use as a personal cleansing agent because they are mild to the skin and produce stable foams. Is usually produced by reacting a saccharide with an excess amount of a higher alcohol with respect to the saccharide, and the reaction product contains unreacted higher alcohol that causes an odor. It needs to be removed.

There are known distillation methods for removing the unreacted higher alcohols and steam distillation method proposed in Japanese Patent Laid-Open No. 3-106895. However, since the boiling point of higher alcohols is generally high, In the distillation method and the steam distillation method, it is necessary to heat at a high temperature, which causes decomposition of the alkyl glycoside, deterioration of hue, etc.
There is a problem in terms of quality.

On the other hand, in Japanese Patent Laid-Open No. 4-13685,
A liquid-liquid extraction method using a non-polar solvent that does not require operation at high temperature has been proposed. Also, for other surfactants, a liquid-liquid extraction method using a non-polar solvent is also used in terms of thermal stability. Purification methods by extraction methods are often used. However, normally, the deterioration of odor and the deterioration of hue are caused by the presence of a very small amount of impurities, but when a small amount (low concentration) of impurities is extracted, the distribution ratio (impurity concentration in extraction solvent / interface) Since the concentration of impurities in the aqueous activator solution becomes small, a large amount of extraction solvent is required, which causes industrial problems such as high cost.

As a method of saving the extraction solvent, there is a method of continuously extracting using a counter-current mixer-settler type extractor, but there is a problem that the apparatus cost becomes high. On the other hand, there is also a method of dispersing the extraction solvent in the surfactant aqueous solution using a perforated plate extraction tower or the like, which has a relatively low equipment cost, but the contact between the surfactant aqueous solution and the extraction solvent is insufficient, so that a large amount of The extraction solvent is required, and the extraction is insufficient.

Therefore, an object of the present invention is to provide an inexpensive apparatus using an extractant (extracting solvent) to remove impurities that cause odor deterioration, hue deterioration, irritation, etc. from an aqueous surfactant solution. It is an object of the present invention to provide a method for producing a surfactant, which can be efficiently extracted and removed by using the same to obtain a high-quality surfactant.

[0008]

Means for Solving the Problems As a result of various studies to achieve the above object, the inventors of the present invention have extracted impurities that cause odor deterioration, hue deterioration, irritation, etc. from an aqueous solution of a surfactant. When extracting and removing with an agent, the aqueous solution of the surfactant and the extractant are continuously countercurrently contacted using an extraction tower, and the aqueous solution of the surfactant is in a dispersed phase (droplet) and the extractant is in a continuous phase. It was found that these impurities can be extracted and removed very efficiently, and many studies have been conducted on the operating method thereof to complete the present invention.

That is, according to the present invention, the components to be extracted are contained from the top of the column of the extraction apparatus having a cylindrical extraction column and a plurality of perforated plates horizontally and vertically arranged in the extraction column. An aqueous solution of a surfactant is supplied, an extractant for extracting the above-mentioned components to be extracted is supplied from the bottom of the tower, and the interface position between the aqueous solution of the surfactant and the extractant is higher than that of the middle porous plate in the porous plate. It is intended to provide a method for producing a surfactant, which comprises a purification step of extracting the above-mentioned components to be extracted while controlling so as to exist below.

The method for producing the surfactant of the present invention will be described in detail below. The extraction device having a cylindrical extraction tower and a plurality of perforated plates horizontally and vertically arranged in the extraction tower used in the present invention includes a reciprocating rotary extraction tower and a rotary disk extraction tower. , A non-rotating perforated plate extraction tower and the like.

Examples of the reciprocating rotary extraction tower, the rotary disk extraction tower and the non-rotating perforated disk extraction tower will be described in detail with reference to FIG. 1 of the accompanying drawings. FIG. 1 (A) is a schematic cross-sectional view showing a reciprocating rotary extraction tower, FIG. 1 (B) is a schematic cross-sectional view showing a rotary disk extraction tower, and FIG. It is a schematic sectional drawing which shows a board | plate extraction tower. Incidentally, FIG.
The rotating disk extraction tower shown in (B) and the non-rotating porous disk extraction tower shown in FIG. 1 (C) are the same as the reciprocating rotary extraction tower, except that they are not described in detail.

A reciprocating rotary extraction tower 10A shown in FIG. 1 (A).
Has a cylindrical extraction tower 1A and a plurality of perforated plates 2A arranged horizontally and vertically in the extraction tower 1A. The perforated plate 2A is the same as that of the extraction tower 1A. The drive shaft 4A extending from the lower edge of the motor 3A installed above is fixed and arranged at a predetermined interval, and the perforated plate 2A faces upward in the peripheral portion. It has a side wall. Since the perforated discs 2A are arranged via the drive shaft 4A, the driving force of the motor 3A can be transmitted to each perforated disc 2A as a rotational force for reciprocating rotational movement in the arrow direction.

A tower top supply port 5A for supplying an aqueous solution of a surfactant is provided at the top of the extraction tower 1A, and a tower bottom supply port 6A for supplying an extractant at the bottom of the tower. , Respectively, and an upper discharge port 7A for discharging the extractant is provided on the upper side of the extraction tower 1A, and a lower part for discharging the aqueous solution of the surfactant is provided on the lower side. Each discharge port 8A is provided.

Rotating disk extraction tower 10B shown in FIG. 1 (B)
Has a cylindrical extraction tower 1B and a plurality of perforated disks 2B arranged horizontally and vertically in the extraction tower 1B, and the perforated disk 2B has a flat disk shape. Has been formed.

Non-rotating perforated plate extraction tower 1 shown in FIG. 1 (C)
0C is a cylindrical extraction tower 1C, and inside the extraction tower 1C,
It has a plurality of perforated discs 2C arranged horizontally and vertically, and each of the perforated discs 2C has an inner wall of the extraction tower 1C so as to alternately have passages through which the continuous phase flows in opposite directions. Fixed to the rim, the non-fixed rim and the extraction tower 1
A predetermined space is provided between the inner wall of C and the inner wall.

The diameter and length of the extraction tower, the diameter of the perforated plate, the number of holes, the plate spacing, the plate number, etc. are not particularly limited, but preferably, the inner diameter of the extraction column is 0.05 to 2 m. The length of the extraction column is 0.5 to 20 m, the diameter of the perforated disc is 0.6 to 0.99 times the inner diameter of the extraction column, the number of holes in the perforated disc is 5 to 10,000, and the step interval of the perforated disc is the inner diameter of the extraction column. 0.2 to 5 times, and the number of stages of perforated plates is 3 to 30. The shape of the perforated plate is shown in FIG.
W type shown in FIG. 1A, flat type shown in FIG. 1B, and FIG.
There are M type etc. shown in. Among them, the W type and the M type have a function of coalescing and further dispersing dispersed phases that descend and rise in the extraction column. Therefore, the W type is preferably used in the present invention.

Among the above extractors, the reciprocating rotary extractor tower can promote the formation of droplets of the dispersed phase by reducing the droplets of the dispersed phase by increasing and decreasing the droplet diameter by increasing and decreasing the droplet diameter of the dispersed phase by reciprocally reversing the porous plate. Furthermore, the area of the extraction interface can be increased, and the extraction efficiency is greatly improved, which is preferable. Examples of the reciprocating rotary extraction tower include a reciprocating rotary liquid continuous extraction tower [manufactured by Shimazaki Seisakusho].
The inversion speed of the perforated plate is preferably 1 to 200 reciprocations / minute.

The aqueous solution of the surfactant used in the purification step in the present invention is an aqueous solution containing the component to be extracted.

The above-mentioned components to be extracted are impurities such as reaction by-products mainly generated when synthesizing a surfactant and unreacted materials of synthetic raw materials, and emit odors such as higher alcohols and higher aldehydes. Alternatively, a coloring substance, a substance having an irritating property, etc. may be mentioned.

The surface active agent may be any of nonionic surface active agents, anionic surface active agents, cationic surface active agents and amphoteric surface active agents. Specific examples of nonionic surfactants include alkyl glycosides, polyoxyethylene alkyl ethers, polyoxyethylene alkylphenol ethers, sorbitan fatty acid esters, and fatty acid monoglycerides.
As the anionic surfactant, higher alcohol sulfate ester salt, fatty acid salt, alkylbenzene sulfonate,
Examples thereof include phosphoric acid ester salts and the like, examples of cationic surfactants include alkylamine salts and quaternary ammonium salts, and examples of amphoteric surfactants include amine oxides and alkyl betaines.

In the present invention, among the above-mentioned surfactants, the following general formula [Chemical formula 3] (the above-mentioned general formula [Chemical formula 1] is used.
The same effect is exhibited when an alkyl glycoside represented by Specific examples of the alkyl glycoside include decyl glucoside, lauryl glucoside, decyl galactoside, lauryl galactoside, decyl fructoside, and lauryl fructoside.

[0022]

[Chemical 3]

The above-mentioned alkyl glycoside is obtained by a well-known method. For example, a method of directly acetalizing a saccharide and a higher alcohol in the presence of an acid catalyst, or a method of previously acetalizing a saccharide with a lower alcohol, It can be prepared by a method of exchanging a higher alcohol with an acetal after forming a lower alkyl glycoside.

Further, in the present invention, among the above-mentioned surfactants, particularly when the amine oxide represented by the following general formula [Chemical formula 4] (the same as the above general formula [Chemical formula 2]) is used, a high effect is obtained. Express. Specific examples of the amine oxide include decyldimethylamine oxide and lauryldimethylamine oxide.

[0025]

[Chemical 4]

The above amine oxide is obtained by a known method, and can be prepared, for example, by a method of oxidizing a tertiary amine with hydrogen peroxide or the like.

The concentration of the surfactant in the aqueous solution of the surfactant is not particularly limited, but is preferably 5% by weight to 60% by weight.

The extractant used in the present invention is preferably a nonpolar solvent having a solubility parameter of 10 or less. For example, n-pentane, n-hexane, n-heptane, n-octane, iso-octane and n-octane. Saturated aliphatic hydrocarbons such as decane; cycloaliphatic hydrocarbons such as cyclohexane, cyclopentane and decalin; aromatic hydrocarbons such as benzene, toluene and p-xylene; carbon tetrachloride; chloroform; petroleum ether and the like, When used, they can be used alone or as a mixture.

The amount of the extractant used is preferably 100 to 10,000 parts by weight, more preferably 100 to 5,000 parts by weight, based on 100 parts by weight of the surfactant. If it is less than 100 parts by weight, the removal rate of the above-mentioned components to be extracted is insufficient, and if it exceeds 10,000 parts by weight, the extraction cost becomes high, which is not industrially preferable.

When there is a tendency for emulsification between the aqueous solution of the surfactant and the extractant, it is preferable to use a demulsifier.

As the demulsifier, a lower alcohol is preferable, and examples thereof include methanol, ethanol, n-propanol, iso-propanol and the like. The amount of the demulsifier used is preferably 10 to 1000 parts by weight with respect to 100 parts by weight of the surfactant.
It is particularly preferable that the amount is ˜300 parts by weight. If it is less than 10 parts by weight, the demulsifying effect may be insufficient, and if it exceeds 1000 parts by weight, the demulsifying effect does not change, which is industrially undesirable. If there is no tendency to emulsify, the demulsifier does not have to be used.

Thus, in the method for producing a surfactant of the present invention, the aqueous solution of the surfactant is supplied from the top of the tower of the extraction device, and the extractant is supplied from the bottom of the tower to remove the surfactant. The method is characterized by having a purification step of extracting the above-mentioned components to be extracted while controlling the interface position between the aqueous solution and the extractant to exist at a specific position. In the present invention, steps other than the above-mentioned purification step, for example, a step of synthesizing a surfactant and the like can be performed according to a conventional method.

In the present invention, the above-mentioned supply of the aqueous solution of the surfactant and the above-mentioned supply of the extractant can be carried out according to a standard method. At this time, the supply amount of the aqueous solution of the surfactant is
0.03 to 30 kg / min, the supply amount of the above extractant is
It is preferably in the range of 0.03 to 100 kg / min.

The specific position where the interface between the aqueous surfactant solution and the extractant is present is a position below the middle porous plate of the plurality of porous plates. Figure 1 shows the specific position
A specific description will be given with reference to (A). In addition, h ₁ is the height between the lowermost perforated plate and the uppermost perforated plate, and h ₂
Is the height from the bottom of the tower to the lowermost perforated plate, and H is the height of the entire tower. And, for h ₁ , h ₂ and H, h ₁
It is preferable to dispose the perforated plate so that the relationships of / h ₂ = 2 to 20 and h ₁ /H=0.4 to 0.9 are established. The specific position is lower than a in FIG. 1 (A) (the position where the middle-stage perforated plate in the height direction of the plurality of perforated plates is present), and preferably the following position:
The following positions are more preferable, and the following positions are particularly preferable. B in FIG. 1 (A) (0.5h from the bottom porous plate)
₁ higher position) and a position higher than the lower discharge port 8A which is the discharge port of the surfactant. C in FIG. 1 (A) (0.3h from the bottom perforated plate)
₁ higher position) and a position higher than the lower discharge port 8A which is the discharge port of the surfactant. A position lower than d (the position where the lowermost porous plate exists) in FIG. 1A and higher than the lower discharge port 8A that is the discharge port of the surfactant.

The following method or the like may be mentioned as a method for controlling the above interface position to the above specific position. Method for controlling the amount of aqueous solution of surfactant extracted Method for controlling the amount of aqueous solution of surfactant supplied

The above method and method will be described below with reference to FIG.
This will be described with reference to (A) and (B). Note that FIG. 2 (A)
FIG. 2B is a schematic view showing an apparatus used when performing the purification step (performing the method) in the present invention, and FIG.
FIG. 3 is a schematic view showing another apparatus used in performing the purification step (performing the method) in the present invention, and
The points which are not described in detail are the same as those in FIG.

In the apparatus shown in FIG. 2 (A), an interfacial meter 11A for measuring the interfacial position 9A is provided below the extraction column 1A (to the bottom of the column), and according to the measurement of the interfacial meter 11A. , Control valve 12A for automatically controlling the opening and closing of the outlet
Is connected to the lower outlet 8A. Then, when the interface position 9A rises, the control valve 12A is opened, the aqueous solution of the surfactant is discharged, and when the interface position 9A descends, the control valve 12A is closed. It can be maintained at a substantially constant position.

In the apparatus shown in FIG. 2B, an interfacial meter 11A for measuring the interfacial position 9A is provided below the extraction column 1A (to the bottom of the column), and the interfacial meter 11A is used for the measurement. , Control valve 12A that automatically controls opening and closing of the supply port
Is connected to the tower top supply port 5A. When the interface position 9A is lowered, the control valve 12A is opened to supply the aqueous solution of the surfactant, and when the interface position 9A is raised, the control valve 12A is closed, so that the interface position 9A is omitted. Can be kept in a fixed position.

In the present invention, as described above, by controlling the interfacial position between the aqueous solution of the surfactant and the extractant to be present at the above-mentioned specific position, the aqueous solution of the surfactant and the extractant flow countercurrently. In the contacting portion, the aqueous solution of the surfactant is used as the dispersed phase (droplets) and the extractant is used as the continuous phase. By making the aqueous solution of the surfactant a dispersed phase (droplet) and the extractant a continuous phase, the contact efficiency between the aqueous solution of the surfactant and the extractant is such that the extractant is a dispersed phase (droplet), the surfactant. It is improved compared with the case where the aqueous solution of is a continuous phase. Hereinafter, regarding this point, FIG.
This will be described in detail with reference to (A) and (B). Here, FIG.
FIG. 3A is a schematic view showing a mode of countercurrent contact when an extractant is a dispersed phase (droplet) and an aqueous solution of a surfactant is a continuous phase, and FIG. It is a schematic diagram showing a mode of countercurrent contact when an aqueous solution is a dispersed phase (droplet) and an extractant is a continuous phase.

When the extractant is the dispersed phase (droplets) and the aqueous solution of the surfactant is the continuous phase, as shown in FIG.
Although the droplet of the extractant 22 rises in the direction of the arrow through the porous plate 2, there is a portion where the aqueous solution 21 of the surfactant cannot come into contact with the droplet of the extractant 22, and the extraction efficiency of the component to be extracted is insufficient. Becomes On the other hand, when the aqueous solution of the surfactant is the dispersed phase (droplet) and the extractant is the continuous phase, the droplets of the aqueous solution 21 of the surfactant are porous as shown in FIG. 3 (B). Since the liquid drops of the aqueous solution 21 of the surfactant all come into contact with the extractant 22 through the board 2 in the direction of the arrow, the extraction efficiency is improved.

In the present invention, the interface means a boundary surface where the continuous phase of the aqueous surfactant solution is in contact with the continuous phase of the extractant [that is, at the interface position shown in FIGS. 2 (A) and 2 (B)). Interface].

In the present invention, the extraction operation temperature is preferably 10 to 60 ° C., and the operation pressure is not particularly limited, but normal pressure is preferable. Further, the extraction can be terminated when the countercurrent contact is terminated and the aqueous solution of the surfactant is lowered to the bottom of the column. In the present invention, the oil agent contained in the aqueous solution of the extracted and purified surfactant and the demulsifier used as necessary (however, the demulsifier may not be used) are removed by a known method such as distillation. can do.

[0043]

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

Example 1 (1) Anhydrous glucose, 5 mol times of n-decyl alcohol to anhydrous glucose, and 0.0035 mol times of paratoluenesulfonic acid to anhydrous glucose were used, The reaction was performed by a known method to obtain a reaction product containing an alkyl glucoside. Then, after removing excess unreacted n-decyl alcohol by distillation at 160 ° C. and 2 mmHg,
The crude alkyl glucoside was obtained by treating it under the conditions of 160 ° C. and 75 mmHg while injecting 2 times the weight of steam with respect to the alkyl glucoside. Next, ion-exchanged water was added to the obtained crude alkyl glucoside to obtain an aqueous alkyl glucoside solution containing 40% by weight of alkyl glucoside. As a result of analyzing the obtained aqueous solution of alkyl glucoside, unreacted n of 800 ppm with respect to the alkyl glucoside
Decyl alcohol remained and had a strong higher alcohol odor.

(2) A mixture obtained by adding and mixing the same amount of ethanol (demulsifying agent) as the alkyl glucoside to the aqueous solution of the alkyl glucoside obtained in (1) above was used. 2 mm, perforated plate diameter 60 m
m, the number of holes in the perforated plate is 22, the step interval is 55 mm, and the number of steps is 8
45 g / m at the tower top supply port 5A of the (W type) reciprocating rotary extraction tower [manufactured by Shimazaki Seisakusho] shown in FIG. 1 (A).
Supplied in. At the same time, n-hexane was supplied from the bottom supply port 6A of the same extraction column at a rate of 300 g / min, and the surfactant was discharged from the lower discharge port 8A and the n-hexane was discharged from the upper discharge port 7A, respectively, to cause countercurrent flow. Continuous extraction was performed. At that time, in order to control the interface position between the aqueous solution of alkyl glucoside and n-hexane to be present 70 mm below the bottom porous plate, the amount of the aqueous solution of alkyl glucoside extracted was adjusted. The perforated plate was reciprocally inverted at 140 reciprocations per minute, the extraction temperature was 45 ° C., and the pressure was normal pressure. Aqueous solution of alkyl glucoside is supplied at the top of the tower 5A
After 30 minutes from the start of supplying the solution, the aqueous solution of alkyl glucoside was sampled from the bottom of the column, and the amount of residual unreacted higher alcohol was measured.
It was 5 ppm. The solvent (n-hexane and ethanol) was distilled off from the resulting purified alkyl glucoside aqueous solution under the conditions of 50 ° C. and 60 mmHg, and the odor was evaluated.

Comparative Example 1 The same amount of ethanol as the alkyl glucoside was added and mixed to the aqueous solution of alkyl glucoside obtained in Example 1 (1), and the mixture was filled with n-hexane in advance to obtain a column diameter of 75. 2 mm, perforated plate diameter 60 mm,
It was supplied to the tower top supply port 5D of the M-type reciprocating rotary extraction tower [manufactured by Shimazaki Seisakusho Co., Ltd.] shown in FIG. Incidentally, FIG.
FIG. 3 is a schematic cross-sectional view showing an M-type reciprocating rotary extraction tower,
The reciprocating rotary extraction tower shown in FIG. 1 (A) is the same as the reciprocating rotary extractor tower shown in FIG. 1 (A) except that the perforated plate is provided upside down. At the same time, n-hexane was added to the extraction tower from the bottom supply port 6D of the extraction tower at 30
Countercurrent continuous extraction was carried out by supplying 0 g / min of the aqueous solution of alkyl glucoside from the lower outlet 8D and extracting n-hexane from the upper outlet 6D, respectively. At that time, the withdrawal amount of the alkyl glucoside aqueous solution was adjusted in order to control the interface position between the aqueous alkyl glucoside solution and n-hexane to be located 70 mm above the uppermost porous plate. In addition, the perforated plate was reciprocally inverted at 140 reciprocations per minute, the extraction temperature was 45 ° C., and the pressure was normal pressure. Thirty minutes after starting the supply of the alkyl glucoside aqueous solution to the tower top supply port 5D, the alkyl glucoside aqueous solution was sampled from the tower bottom and the residual unreacted higher alcohol content was measured.
It was pm. From the obtained purified alkyl glucoside aqueous solution, the solvent (n-hexane and ethanol) was distilled off under the conditions of 50 ° C. and 60 mmHg, and the odor was evaluated.

Example 2 (1) Lauryldimethylamine, 0.5 mol times citric acid with respect to lauryldimethylamine, 1.05 mol times hydrogen peroxide with respect to lauryldimethylamine, and lauryldimethylamine On the other hand, 1.55 times by weight of ion-exchanged water was used to carry out the reaction by a known method to obtain an aqueous solution containing 35% by weight of lauryldimethylamine oxide.
When the odor of this aqueous solution was evaluated, there was a strong higher aldehyde odor.

(2) A mixture of 100 parts by weight of the lauryldimethylamine oxide aqueous solution obtained in (1) and 30 parts by weight of ethanol was mixed with n-hexane in Example 1 (2). The same reciprocating rotary extraction tower was supplied to the top supply port 5A at 95 g / min. At the same time, n-hexane was added to the bottom of the extraction tower at the bottom supply port 6A.
Was supplied at a rate of 105 g / min, and countercurrent continuous extraction was performed by extracting the lauryldimethylamine oxide aqueous solution from the lower outlet 8A and the n-hexane from the upper outlet 7A, respectively. At that time, in order to control the interface between the aqueous lauryldimethylamine oxide solution and n-hexane so as to exist 70 mm below the lowermost porous plate, the amount of the aqueous lauryldimethylamine oxide solution withdrawn was adjusted. Further, the perforated plate was reciprocally inverted at 100 reciprocations per minute, the extraction temperature was 50 ° C., and the pressure was normal pressure. Thirty minutes after starting the supply of the lauryldimethylamine oxide aqueous solution to the tower top supply port 5A, the lauryldimethylamine oxide aqueous solution was sampled from the tower bottom at 50 ° C.,
Solvent (n-hexane and ethanol) under the condition of 60 mmHg
When the odor was removed and the odor was evaluated, there was almost no higher aldehyde odor.

Comparative Example 2 A mixture of 100 parts by weight of the aqueous lauryldimethylamine oxide solution obtained in Example 2 (1) and 30 parts by weight of ethanol was prepared in advance.
It was supplied to the tower top supply port 5D of a reciprocating rotary extraction tower similar to Comparative Example 1 filled with hexane at 95 g / min. At the same time, n-hexane was supplied at a rate of 105 g / min from the tower bottom supply port 6D of the same extraction tower, and the lauryldimethylamine oxide aqueous solution was supplied from the lower discharge port 8D to n-hexane.
Countercurrent continuous extraction was performed by extracting hexane from each of the upper outlets 7D. At that time, in order to control the interface between the aqueous lauryldimethylamine oxide solution and n-hexane so as to exist 70 mm above the uppermost porous plate, the extraction amount of the aqueous lauryldimethylamine oxide solution was adjusted. Further, the perforated plate was reciprocally inverted at 100 reciprocations per minute, the extraction temperature was 50 ° C., and the pressure was normal pressure. Thirty minutes after starting supplying the lauryldimethylamine oxide aqueous solution to the tower top supply port 5D, the lauryldimethylamine oxide aqueous solution was sampled from the tower bottom, and the solvent (n-hexane and ethanol) was distilled off under the conditions of 50 ° C. and 60 mmHg. When the odor was evaluated, there was a slightly strong higher aldehyde odor.

Table 1 shows the measurement results of the aqueous surfactant solutions obtained in Examples 1 and 2 and Comparative Examples 1 and 2.

[0051]

[Table 1]

[0052]

EFFECTS OF THE INVENTION According to the method for producing a surfactant of the present invention, impurities that cause deterioration of odor, deterioration of hue, irritation, etc. are extracted from an aqueous solution of a surfactant using an extractant at low cost. It is possible to efficiently extract and remove using a different device, and obtain a surfactant of extremely high quality.

[Brief description of drawings]

1 (A) is a schematic sectional view showing a reciprocating rotary extraction tower, FIG. 1 (B) is a schematic sectional view showing a rotary disk extraction tower, and FIG. 1 (C) is It is a schematic sectional drawing which shows a non-rotating perforated plate extraction tower.

FIG. 2 (A) is a schematic view showing an apparatus used for carrying out the purification step in the present invention, and FIG.
FIG. 3 is a schematic view showing another apparatus used when performing the above-mentioned purification step in the present invention.

FIG. 3 (A) is a schematic view showing a mode of countercurrent contact when an extractant is a dispersed phase (droplet) and an aqueous solution of a surfactant is a continuous phase, and FIG. FIG. 4 is a schematic view showing a mode of countercurrent contact when an aqueous solution of a surfactant is used as a dispersed phase (droplet) and an extractant is used as a continuous phase.

FIG. 4 is a schematic sectional view showing an M-type reciprocating rotary extraction tower.

[Explanation of symbols]

 1A Extraction Tower 2A Porous Plate 3A Motor 4A Drive Shaft 5A Tower Top Supply Port 6A Tower Bottom Supply Port 7A Upper Discharge Port 8A Lower Discharge Port 9A Interface Position 11A Interface Meter 12A Control Valve 21 Surfactant Solution 22 Extractant

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁵ Identification code Internal reference number FI technical display area C11D 1/75

Claims (4)

[Claims] 1. A surfactant containing a component to be extracted from the top of an extraction apparatus having a cylindrical extraction tower and a plurality of perforated plates horizontally and vertically arranged in the extraction tower. An aqueous solution is supplied, and an extractant for extracting the components to be extracted is supplied from the bottom of the tower, and the interface position between the aqueous solution of the surfactant and the extractant is lower than the middle porous plate in the multiple porous plates. A method for producing a surfactant, comprising a purification step of extracting the above-mentioned components to be extracted while controlling the above. 2. The method for producing a surfactant according to claim 1, further comprising supplying 10 to 1000 parts by weight of a demulsifier with respect to 100 parts by weight of the surfactant. 3. The surfactant is represented by the following general formula:
Or an alkyl glycoside represented by the following general formula [Chemical formula 2]
The method for producing a surfactant according to claim 1, which is an amine oxide represented by: [Chemical 1] [Chemical 2] 4. The method for producing a surfactant according to claim 1, 2 or 3, wherein the perforated plate is reciprocally rotated.