WO2006009320A1

WO2006009320A1 - Process for production of powdery n-(long-chain acyl)- amino acids or salts thereof, powdery n-(long-chain acyl)amino acids or salts thereof, and facial cleansing powders

Info

Publication number: WO2006009320A1
Application number: PCT/JP2005/013891
Authority: WO
Inventors: Yoshinori Yamaguchi; Satoshi Ueda; Makoto Nishikawa
Original assignee: Ajinomoto Co., Inc.
Priority date: 2004-07-23
Filing date: 2005-07-22
Publication date: 2006-01-26

Abstract

A process for mass-producing continuously powdery surfactants suitable for detergents or cosmetic ingredients, particularly for facial cleansing powder. This process is characterized by comprising the step of conducting the size reduction of a surfactant consisting of an N-(long-chain acyl)amino acid or a salt thereof by pulverizing the surfactant by the use of either a roll mill or equipment having a pulverization mechanism of discharging a material fed into the clearance between a rotary vane and a mesh plate placed around the periphery of the vane through openings of the mesh plate. According to the invention, N-(long-chain acyl)amino acids or salts thereof can be pulverized without extra heating or cooling the acids or salts (powder before pulverization) or adding a pulverization aid to the acids or salts to attain the size reduction of the acids or the salts with substantially no impairment in the powder characteristics (such as bulk density and water content) inherent in the acids or salts (powder before pulverization). Thus, the invention enables industrial continuous mass production of powdery N-(long-chain acyl)amino acids or salts thereof capable of giving facial cleansing powders which are free from coarseness in washing hands and little cause dusting.

Description

Specification

Powdered N_long chain acylamino acid or a salt thereof, powdered N—long chain acylamino acid or a salt thereof, and face washing powder

Technical field

The present invention provides a powdery N-long chain acylamino acid or a salt thereof which enables continuous mass production of a powdery N-long chain acylamino acid or a salt thereof preferable as a raw material component for washing lj, cosmetics and the like. The present invention relates to a method for producing a salt, and also relates to a powdery N-long chain acylamino acid or a salt thereof and a powdered N-long chain acylamino acid or a salt thereof particularly suitable as a raw material component of the facial powder.

Background technology

Surfactants are used as raw material components for various washings and cosmetics, and are prepared in liquid or solid form according to their properties and applications. A powdery surfactant is known as one of the solid surfactants. The powdery surfactant is mainly used as a powder cleaning agent for facial cleansing powder, soap powder, etc. It is used as a liquid washing agent dissolved in a liquid such as body shampoo.

Conventionally, spray dryer products have been known as such powdery surfactants. When the spray dryer is adjusted in particle size (particle size) according to its operating conditions, it is the moisture content of the powder. It also affects the powder physical properties other than the particle size (particle size) such as bulk density, and it is difficult to adjust the powder physical properties of only the particle size. It is not easy, and powders produced by spray dryers generally tend to have a low bulk density and are prone to dusting. Thus, for example, it is conceivable to granulate a spray-dried product once to reduce powder formation. As a pulverization method for various substances, a method of pulverization while cooling with dry ice or liquid nitrogen is known (Chemical Engineering Handbook 6th edition, P838). Such cooling powder is not suitable for continuous operation because of the amount of work and cost, and is not suitable for industrial mass production.

In addition, in order to knead the surfactant particles with a powder builder of a specific particle size to increase the hardness (to a kneaded product of a specific hardness) and to grind, or to obtain a detergent with a high bulk density, A method has been proposed in which a grinding aid such as light is kneaded, and the resulting kneaded product is aired at 15 to 20 ° C. and cooled while being cooled (Japanese Patent Laid-Open No. 9-2 3 5 5 No. 98, JP-A-10-88197, etc.), and this method cannot be obtained as a powder of a surfactant alone. Therefore, there is a need for a method capable of industrially mass-producing powdery surfactants with improved strength and powderiness.

Powdered surfactants, especially face-washing powders, are required to have properties such as no gritty feel when hand-washed and less dusting. Development of such powdery surfactants is desired. ing. However, as described above, conventionally, a powdery surfactant is not known as a spray dryer product, and therefore, in order to obtain a powdery surfactant suitable for a facial cleansing powder, a spray is required. There has been proposed a method of removing fine particles that cause powder formation by sieving the powder obtained with a dryer (Japanese Patent Laid-Open No. 2 0 3-3 0 6 6 9 6). Since particles with a particle size of less than 0.05 mm are sieved, the clogging of the sieve is unavoidable in long-term operation, and the sieve is frequently washed to process a large amount of powder. Therefore, this technology is not necessarily suitable for industrial mass production. Accordingly, there is an urgent need for a process for producing a powdery surfactant capable of continuous mass production in order to obtain a powdery surfactant suitable for a face washing powder.

Disclosure of the invention

The present invention has been made in view of the circumstances as described above, and the problem to be solved is a powdery surfactant preferable as a raw material component of cosmetics and the like, and particularly suitable as a raw material component of a facial cleansing powder. A powder that can achieve a face washing powder that is strong and resistant to powdering, without the gritty feeling of hand-washing. The purpose is to remove the surface active agent.

As a result of intensive studies to solve the above-mentioned problems, the present inventors pulverized N-long chain acylamino acid or a salt thereof using a specific pulverization facility, thereby applying extra heat or cooling. Without the need to add pulverization aids, and the fact that the particle size can be reduced without substantially affecting the powder physical properties such as bulk density and moisture content. By overlapping, the present invention has been completed. That is, the present invention

(1) A method for producing a powdered N-long chain acylamino acid or a salt thereof, characterized by being subjected to a step of pulverizing N-long chain acylamino acid or a salt thereof with a kneader.

(2) The Ronore mill has one or more gear-shaped rolls on the surface, and the pitch width of the gear in the first stage is equal to or greater than the cumulative 30% particle diameter of the feed powder, and the cumulative 95% particle The method according to (1) above, which is not more than the diameter,

(3) The clearance between one and the other in each step of a single step or multiple steps is 0.12 times the pitch width of the gear on the surface, 1 The method described in (2) above,

(4) The method according to (2) or (3) above, wherein the pitch width of the gear on the surface of the last stage mouthpiece is 0.35 mm or less,

(5) Ronole mill has one or more rolls with a smooth surface and the clearance between one and the other roll of the first stage roll is more than 30% of the cumulative particle size of the feed powder. The method according to (1), wherein the particle size is 95% or less,

(6) One of the above-mentioned (2) to (5), wherein the rotation speed ratio of one roll to the other roll in each roll of a single roll or multiple rolls is 1.0 to 1.8. The method described in

(7) The method according to (5) or (6) above, wherein the clearance of the final roll is 0.35 mm or less,

(8) N-long chain acyl amino acid or a salt thereof before pulverization is a powder having a force density of 0.4 gZcm ³ or more and a particle content of less than 10 106 mm and less than 10%. The method according to any one of the above (1) to (7),

(9) N-long chain acylamino using a facility equipped with a crushing mechanism that discharges the material supplied to the gap between the rotor blade and the mesh plate arranged on the side of the rotor blade from the mesh hole of the mesh plate A process for producing a powdered N-long chain acylamino acid or a salt thereof, characterized by being subjected to a step of pulverizing an acid or a salt thereof;

(10) The method according to (9) above, wherein the mesh hole diameter of the mesh plate is 0.25 to 2 times the cumulative 90% particle diameter of the feed powder, (11) The method according to (9) or (10) above, wherein the clearance between the rotor blades and the mesh plate is 0.01 to 5 mm,

(12) N-long chain acyl amino acid or a salt thereof before flour has a content of particles having a force density of 0.4 g / cm ³ or more and a particle size of 0.1 106 mm or less. /. The method according to any one of the above (9) to (: L 1), which is a powder of less than

(13) The material is supplied to a gap between the rotary blade and the mesh plate arranged on the side circumference of the rotary blade, and is pulverized by a facility equipped with a powder stone mechanism that discharges the mesh plate from the mesh hole. The method according to any one of the above (1) to (12), further comprising a step of fluidizing and coagulating the powder of N-long chain acylamino acid or a salt thereof obtained to increase the particle size ,

(14) at a content of the particle diameter 0. 106 mm or less of the particles is less than 10%, does not contain particle diameter 0. 355 mm or more particles in a bulk density of 0. 4 g ^ cm ³ or more powder Powdered N-long chain acylamino acid or a salt thereof, characterized in that

(15) A face-washing powder comprising the powdery N-long chain acylamino acid or salt thereof according to (14) above, and

(16) The present invention relates to a face-washing powder characterized by containing a powdery N-long-chain acylamino acid or a salt thereof produced by the method described in (4) or (7) above. According to the present invention, N-long amino acid or a salt thereof (powder) can be pulverized without substantially changing powder physical properties such as bulk density and moisture content. Therefore, for example, it is suitable as a raw material component of a lath and washing powder that has a high bulk density but does not substantially contain coarse particles and has a very small content of fine particles that cause dusting. A powdery N-long chain acyl amino acid or a salt thereof can be produced continuously.

In addition, according to the present invention, it is possible to obtain a powdered N-long chain acyl amino acid or a salt thereof that can give a facial cleansing powder that does not feel rough when hand-washed and does not easily cause powdering. .

BEST MODE FOR CARRYING OUT THE INVENTION

Hereinafter, the present invention will be described in more detail. The N-long chain acylamino acid used in the present invention is synthesized by a known method such as adding a fatty acid quinolide to an amino acid alkali solution. The N-long chain acyl amino acid may be a single compound or a mixture of two or more compounds having an acyl group with different chain lengths. As the acyl group, for example, a saturated or unsaturated linear or branched aliphatic acyl group having 6 to 18 carbon atoms can be used. For example, hexanoyl, otanoinore, decanol, lauroyl, myristoylet, Examples include acyl groups such as panoremitoinole, stearoinole and oleoyl. It may also be a mixed acyl group such as coconut oil fatty acid acyl, palm kernel oil fatty acid acyl, and hardened beef tallow fatty acid acyl. The type of amino acid constituting the N-long chain acyl amino acid is not particularly limited, and examples thereof include glutamic acid, glutamine, aspartic acid, asparagine, glycine, and alanine, and the desired N-long chain amino acid or From the viewpoint of fluidity and cost of the powder of the salt, glutamic acid, glycine and alanine are preferable, and glutamic acid is particularly preferable. As the amino acid constituting the N-long chain acylamino acid, an optically active substance, an arbitrary mixture of enantiomers, or a racemate may be used.

The type of the N-long chain acyl amino acid salt is not particularly limited, and can be appropriately selected from salts usually used in the art. For example, alkali metal salts such as sodium salt and potassium salt, alkaline earth metal salts such as calcium salt and magnesium salt, metal salts such as ammonium salt and zinc salt, ammonium salt, monoethanolamine salt, diethanolamine salt, triethanolamine salt Examples include organic amine salts such as ethanolamine salts, salts of basic amino acids such as arginine salts and lysine salts. From the viewpoint of the solubility of the salt, an alkaline metal salt or an alkaline metal salt is preferred, and an alkaline metal salt is particularly preferred.

In the present invention, one or more N-long chain acyl amino acids or salts thereof can be used as the N-long chain acyl amino acids or salts thereof to be subjected to pulverization.

In addition, the kneading mill used in the present invention may be one having a structure in which the powder supplied between a pair of rotating knurling is ground by being compressed and sheared, and should be pulverized. N—Method for supplying long-chain acyl amino acids or their salts Method) may be a method of feeding at a constant speed between a pair of rotating rolls, variable feeding, or intermittent feeding. However, the change in the supply speed leads to a change in the density of the powder passing between the rolls. When the density is high, the contact frequency between the powder and the powder increases, and the pressure on the force powder also increases. Therefore, pulverization is easier to proceed and the particle size of the powder is smaller than when the fineness is low. Therefore, from the standpoint of continuously producing products with the same particle size distribution for a long time, it is desirable to supply them at a constant speed using a screw feeder or the like.

Although the feed rate of the long-chain acylamino acid or salt thereof to the kneading mill depends on the girdle rotation speed, it is usually preferred to feed at 20 kg / hr / cra-kall or less. When the feed rate is higher than that of 20 kg / hr m -roll, heat generation due to overloading of the pulverizer increases, causing adhesion and softening of N-long chain acyl amino acids and their salts. From the viewpoint of continuous stability of 1 $, the feeding rate of N-long chain amino acid or its salt to the roll mill is preferably 15 kg / hr / cm-roll or less, and 13 kg / hr / cm-roll or less. Is more preferable. However, the lower limit of the feed rate is preferably 1 kg / hr / cra-mol or more from the viewpoint of production efficiency. _{C In the} present invention, the N-long chain acylamino acid or feed to the roll mill (feed) The particle diameter of the salt is not particularly limited. This is because powders with various particle sizes can be handled by adjusting the clearance and pitch width of the roll. On the other hand, the particle shape of the powder preferably has an aspect ratio (long side / short side) <10. If the aspect ratio (long side / short side) is 10 or more, the particle orientation force when passing between rolls may greatly affect the particle size of the product (pulverized powder). . From the viewpoint of controllability of the particle size of the resulting product and prevention of heat generation and adhesion due to local overload, the aspect ratio (long side / short side) of the powder particles is more preferably 8 or less. The following are particularly preferred:

The clearance of the above-mentioned mouth is the gap width between one mouth and the other mouth, and the pitch width is the unevenness of the mouth-nose surface in a gear shape. This is the distance between mountains when they are held. The aspect ratio (long side / short side) of the powder particles is 2 mg of the powder, and the aspect ratio of the individual particles constituting the powder 2 g is determined by microscopic observation. It is an average value obtained by actually measuring and calculating the average value. In the present invention, the water content of the N-long chain acyl amino acid or salt thereof (powder before pulverization) fed to the roll mill is not particularly limited, but is 10% or less from the viewpoint of preventing increase in the viscosity of the powder. It is preferably 8.5% or less. If the water content exceeds 10%, it becomes easy to become clayey powder or roll adhesion, and the resulting product tends to be plate-like and tends to remain rough. .

It is preferable that a roll at each stage of the roll mill used in the present invention is provided with a scraping blade for scraping off the adhering powder, and a gap width (separation distance) between the roll and the scraping blade. Is preferably 0.0 mm to 0.1 mm. When the width exceeds 0.1 mm, the raw material powder gradually adheres to the Rhono surface due to a continuous long time of 31 $, and when this adhesion grows, the clearance between the rolls becomes narrower. The particle size of the powder) may change over time, so that it is preferable. Further, if the width is less than 0.01 mm, the blade may come into contact with the Rhono surface, and the blade may be chipped and mixed into the product (powdered powder). In particular, from the viewpoint of controlling the particle diameter of the product (powdered powder), the width is more preferably 0.05 to 0.08 mm, and 0.08 to 0.06 mm. Further preferred.

The number of stages in the roll mill used in the present invention is not particularly limited, and may be one stage or a plurality of stages, preferably a plurality of stages. This is because if there is a large body in the feed powder (powder before pulverization) or the raw material (powder before pulverization) particle size and product, When there is a large difference in the particle size (target value) of the (pulverized powder), the adhesion to the roll becomes intense, and the concentration causes overload, and it is stretched into the product (pulverized powder). This is because it may be easy to form a plate-like particle. When a large amount of plate-like particles are formed in the product (powder after powdering), it becomes easy to cause a problem that a rough feeling remains when washing hands. In addition, when only one roll is used, the particle size distribution of the resulting product (powdered powder) tends to be wide, resulting in coarse particles that cause a rough feeling when washing hands and fine particles that cause dusting. It becomes easy. Therefore, it is preferable to provide two or more rolls in series so that the coarse powder is pulverized in stages, and three stages are particularly preferable. The surface of the roll in the roll mill may be a smooth surface, but preferably has gear-like irregularities from the viewpoint of further improving the controllability of the particle diameter. When the surface is a smooth surface, the resulting product tends to be mixed with a finely pulverized product, which is compacted and formed into flakes. When the roll mill has a plurality of rolls, it is preferable that each roll of the plurality of rolls is constituted by a roll having gear-like irregularities: the roll mill roll is a roll having gear-like irregularities on the surface thereof. In some cases, the pitch width of the gear on the tool surface (gap between the crests of the gear) should be within the range of 30% or more and 95% or less of the particle size of the raw material (powder before pulverization). It is preferable. If the pitch width is less than the cumulative 30% particle diameter of the raw material (powder before powder), the equipment will be overloaded, and adhesion due to heat generation will easily occur, and if the cumulative particle diameter exceeds 95%, The particle size does not change much before and after the powder kneading, which is not preferable from the viewpoint of grinding efficiency. From the viewpoint of more stable il, the pitch width is preferably within the range of 40% or more cumulative particle diameter of raw material (powder before powder), 95% or less of cumulative particle diameter, and more than 50% cumulative particle diameter. A value within the range of 95% cumulative particle size or less is particularly preferable.

Further, the pitch width is preferably set in the range of 0.7 times or more and 1.3 times or less of the desired maximum particle size of the product (pulverized powder). In this way, the maximum particle size of the product (powdered powder) is roughly adjusted to the desired value with the pitch width of the gear-like irregularities on the roll surface, and fine adjustment of the maximum particle size and particle size distribution are achieved by clearance. Adjusted. If the pitch width is less than 0.7 times or exceeds 1.3 times, fine adjustment by clearance becomes difficult, which is not preferable.

From the viewpoint of more stable and continuous production of products with desired powder properties, the raw material (powder before powder frame) is pulverized stepwise by using ^two stages of rolls with gear-like irregularities on the roll surface. In this case, the pitch width of the gear-shaped irregularities on the surface of the first stage mouthpiece is 30% or more of the cumulative particle size of the raw material (powder before powdering) and 95% or less of the cumulative particle size. Within the lower range, the pitch width of the gear-shaped irregularities on the first surface of the second stage mouthpiece is 0.7 times or more the desired maximum particle size (target value) of the product (powdered powder), It is preferable to set within the range of 1.3 times or less. More preferably, the pitch width of the gear-like irregularities on the surface of the first stage mouthpiece is equal to or greater than the cumulative 40% particle diameter of the raw material (powder before pulverization) and the cumulative 95% particle It is preferable that the particle diameter is within the range of 50% or less of the particle diameter, and 95% or less of the particle diameter.

Using three stages of Ronoré will enable more stable continuous operation. In this case, the pitch width of the second stage roll is set within the range of 20% or more of the raw material (pre-ground powder) cumulative particle diameter and 85% or less of the cumulative particle diameter, and the pitch width of the third stage roll is the product. It is preferable to be within the range of 0.7 times or more and 1.3 times or less of the desired maximum particle diameter (target value) of the (pulverized powder).

The clearance of the roll of the roll mill used in the present invention is not particularly limited. However, when using a roll with a roll-like uneven surface, it is usually at least 0.12 times the pitch width and 1 times the pitch width. It is set within the following range. If the clearance is less than 0.12 times the pitch width, the effect of the clearance on the particle diameter of the product (pulverized powder) becomes large, and a lot of fine particles are generated in the product. However, it is not preferable because the product tends to be consolidated into plate-like particles. On the other hand, when the clearance exceeds 1 times the pitch width, it is not preferable because a large number of particles pass without being crushed by a pair of rolls and being crushed. Therefore, from the viewpoint of particle size control, the clearance of the mouth is preferably 0.15 times or more of the pitch width and more than 1 time of the pitch width, particularly preferably 0.18 times or more and 1 time or less. .

When the roll surface is a smooth surface, the roll clearance is preferably not more than the desired maximum particle size (target value) of the product (pulverized powder). In addition, as in the case of using a roll having a roll-like irregularities on the roll surface, from the viewpoint of more stably and continuously producing a product with desired powder physical properties, it is stepwise with two or more rolls. In this case, the clearance of the first stage mouth should be within the range of more than 30% particle diameter of the raw material (powder before pulverization) and less than 95% particle diameter. It is preferable to set the clearance of the mouthpiece to the desired maximum particle size (target value) of the product (powdered powder). In order to perform a more stable continuous operation, it is preferable that the pitch width of the first stage gate is within the range of 40% particle diameter or more and 95% particle diameter or less, and 50% particle accumulation. More preferably, the particle diameter is within the range of not less than the diameter and not more than the cumulative 95% particle diameter. Furthermore, it is more desirable to use three stages of the mouthpiece, and the clearance of the second stage is the cumulative 20% particle size of the raw material. As described above, it is more preferable to set the cumulative particle size to 85% or less and set the third step pitch width to the desired maximum particle size (target value) of the product (pulverized powder).

In the present invention, the number of rotations of the roll of the roll mill is not particularly limited, but since the feed flow rate can be increased as the number of rotations increases, the pulverization processing speed is increased, which is effective. However, the rotation speed ratio of the pair of rolls (high-speed rotation roll rotation speed / low-speed rotation roll rotation speed) is usually set in the range of 1 to 1.8. If the powder to be crushed and powdered has a strong softening property and adherence is strong, the particles of the resulting product (powdered powder) are stretched only by using the compression action of crushing with a pair of rolls. In order to reduce the formation of flake particles as much as possible even for powders that are prone to flakes and have strong adhesion, the shearing action is effectively reduced by varying the degree of rotation of the pair of rolls. It is preferable that the rotation speed ratio is 1.2 or more in order to make effective use of the shearing action. However, if the rotation speed ratio of a pair of rolls becomes too large, not only will the balance as rotation β become unstable and unstable, but also the cutting action will work more strongly than the compression action, and the resulting product (powdered powder) The particle diameter of the body is reduced by the pitch width and the tally balance, and the particle diameter control force S becomes difficult. Therefore, the rotational speed ratio needs to be 1.8 or less. Further, from the viewpoint of avoiding heat generation and softening of the powder to avoid adhesion as much as possible, 1.6 or less is preferable. The following is more preferable.

When producing powder for facial cleansing powders of long-chain acylamino acids or their salts by this method, use a roll with irregularities with gear-like surfaces, and increase the pitch width of the final stage tool. It is preferable to be 0.35 mm or less. If the pitch width of the final roll exceeds 0.35 mm, the resulting product (powdered powder) will generally have a large particle size and will tend to feel rough. In addition, from the viewpoint of hand washing feeling, the product (powdered powder) preferably does not contain particles with a particle size exceeding 0.33 mm, and does not contain particles with a particle size exceeding 0.3 O mm. Particularly preferred. Accordingly, the pitch width of the final roll is more preferably 0.33 mm or less, and particularly preferably 0.30 mm or less. If the pitch width of the roll in the final stage is too small, the resulting product (powdered powder) will have a small particle size as a whole and cause powdering. Therefore, the pitch width of the final roll is 0.16 m. m or more is preferable, and 0.150 mm or more is more preferable. Note that the term “staged mouthpiece” as used herein refers to the concept including the first stage mouthpiece in the case of a mouth mill consisting of one stage mouthpiece.

From the same viewpoint, even when a roll having a smooth surface is used, the upper limit of the clearance of the final roll is preferably 0.35 mm or less, more preferably 0.33 mm or less, and 0.3 O mm or less is particularly preferable, and the lower limit is preferably 0.16 mm or more, more preferably 0.15 O mm or more.

The mouth-no-minole used in this paper is not particularly limited as long as it is a facility equipped with a mechanism capable of directly compressing and shearing an N-long chain acyl amino acid or its salt by the rotation of a pair of opposite mouth-to-mouth. Although known equipment can be used, preferred examples include a roll durailleur (manufactured by Nippon Granulator Co., Ltd.), a multistage roll mill (Sanyo Trading Co., Ltd., C PM¾fc $ ¾, roll crusher (Danoretonne: fc $ ¾ In the present invention, there is provided a powder storage mechanism for discharging the material supplied to the gap between the rotor blade and the mesh plate arranged on the side periphery thereof, not the mouth mill, from the mesh hole of the mesh plate. The desired powdery 連続 -long-chain acylamino acid or its salt can be continuously produced using the equipment (ie, comil (quadrone ring, trade name) type powder mash equipment). In this case, the mesh hole diameter of the mesh plate in the equipment is 0.25 times the cumulative 90% particle diameter of the long-chain acylamino or its acid salt powder raw material (pre-ground powder). As described above, it is preferably set within a range of 2 times or less, and if the mesh pore diameter is less than 0.25 times, it is not preferable because the powder stone hoe is overloaded and the mesh is easily clogged. If the number exceeds twice, the number of particles passing through without being dusted increases, which is not preferable from the viewpoint of dusting efficiency, from the viewpoint of more efficient and safer continuous use in actual production. The mesh pore size is more preferably within the range of 0.3 to 1.5 times the cumulative 90% particle size of the pulverized raw material (pre-powder powder), 0.3 to 5 times, A range of 1.6 times or less is particularly preferable.

In addition, the clearance (gap width) between the rotor blades and the mesh plate in the gap between the rotor blades and the mesh plates arranged on the side (granulation region) is not less than 0.1 mm and not more than 5 mm. Within the range is preferable. If it is less than 0.0 l mm, the pulverized raw material (powder before pulverization) is kneaded into the mesh. It is not preferable because it tends to clog and the resulting product tends to become a kneaded rod. On the other hand, if it exceeds 5 mm, the powdered raw material (powder before pulverization) will not be pulverized and it will be easy to circulate through the talari- sion part. In actual production, the clearance is more preferably in the range of 0.05 mm or more and 3 mm or less, more preferably 0.1 mm or more from the viewpoint of more effective and safer continuous 11 hours. The range of 2 mm or less is particularly preferable. The shape of the powder stone structure in the equipment is not particularly limited, but it has an inverted conical shape compared to the type in which the mesh plate arranged on the side circumference of the rotor blade is cylindrical (that is, The diameter of the end on the powder supply side is large, and the diameter gradually decreases toward the end opposite to the end). As such a device, there is QUADRO C0MIL (manufactured by Paulek).

In the present invention, by using a milling machine of a roll mill or combil (quadrone; ^, trade name) type, N-long chain acyl amino acid or a salt thereof (powder before powdering) is ground, Can the particle size of the powder be reduced without substantially affecting the powder physical properties such as moisture content (ie, while minimizing fluctuations in the powder physical properties)? (I) A powdery N-acylamino acid or salt thereof having powder properties preferable as a raw material for cosmetics and the like can be continuously mass-produced. As N-acylaminoic acid or its salt (powder before pulverization) used for pulverization, powders obtained by various production methods (drying method, fine pulverization method) can be used. From this viewpoint, it is preferable to use a powder having a bulk density of 0.4 g Z cm ³ or more. That is, by using a powder having a strength density of 0.4 g / cm ³ or more, the particles that cause powdering are limited to particles having a smaller particle diameter. Specifically, by using a powder having a bulk density of 0.4 g Z cm ³ or more, the content of particles having a particle size of 0.16 mm or less is less than 10% by weight. By crushing to a fine powder, it is possible to obtain a powder that is less prone to dusting. The more effectively suppress dusting, bulk density before milling powder 0. 4 5 cm ³ or more, more preferably, 0. 5 0 cm ³ or more is particularly preferable. Further, the powder before pulverization has a particle size of less than 0.16 mm and contains less than 10% (preferably 9.0 ° / ₀ , more preferably 8.0%). In the case of a body, the content of particles having a particle diameter of 0.16 mm or less is 10 wt. /. Less than products (powdered powder) can be obtained It is preferable. If the bulk density of the powder before pulverization is too large, the particle hardness of the product obtained by pulverization (powder after pulverization) becomes high, and it becomes easy to feel a rough feeling during hand washing. Therefore, the upper limit of the bulk density is preferably 0.80 g / cm ³ or less, and more preferably 0.70 gZ cm ³ or less.

According to the method of the present invention, it is possible to obtain a powdery N-acylamino acid or a salt thereof for facial cleansing powder that does not feel a rough feeling during hand washing, and that is hard to generate powder. Power can also be continuously mass-produced. Powdered N-amino acid or its salt for face-washing powder that does not feel such a rough feeling when washing hands and is less prone to dusting, has a particle size of 0.16 mm or less. It is specified as a powder with a content of less than 10%, no particles with a particle size of 0.355 mm or more, and a strength density of 0.4 g / cm ³ or more.

The powder has a particle content of 9.06 mm or less and a content of 9.0. /. In the following, when the content is 8.0% or less, it is more preferable that powdering is less likely to occur. Note that if the bulk density of the powder becomes too large, the particle hardness tends to be high, and a rough feeling tends to be felt. Therefore, the upper limit of the bulk density of the powder is preferably 0.80 gZcm ³ or less, and more preferably 0.70 g / cm ³ or less.

In the method of the present invention, the powder of N-long chain acylamino acid or a salt thereof is pulverized so that the particle properties of the powder, such as bulk density and moisture content, are not substantially affected. It is possible to reduce the particle size by reducing the particle size by continuously reducing the particle size and producing a large amount of powdered N-acylaminoic acid or its salt that has favorable powder properties for raw materials such as detergents and cosmetics. It is also possible to increase the particle diameter to a desired range by fluidizing the powder. For example, it is desirable that the surfactant in the face-washing foam has an average particle size (cumulative 50% particle size) force SO. 500 mm or more. However, powdered N-long chain acyl amino acids or salts thereof for face-washing foams are preferred. When the powder is manufactured, it is possible to easily increase the average particle size (cumulative 50% particle size) to 0.500 mm or more by using the fluidized granulation method.

In the present invention, the average particle size (cumulative 50% particle size) of the product (powdered powder) varies depending on the specific use of the product (powdered powder). It is preferably within the range of 0.16 mm or more and less than 0.35 5 mm, more preferably 0.15 Omm or more, 0.35 5 mm, or less.

In addition, after N-acylamino acid or a salt thereof is pulverized using a roll mill or Comil type pulverizing equipment, the obtained powder is fluidized by a fluid granulation method or the like to increase the particle size thereof, and the face washing foam In the case of producing a powder for use, the average particle size after accumulation (cumulative 50% particle size) is preferably 0.500 mm or more, particularly preferably 0.500 mm or more, 5.0 0 O It is desirable that the bulk density is 0.8 mm / cm ³ or less.

In the present invention, the product, that is, the powder after pulverization, and the powder obtained by further flowing the powder after pulverization by a fluidized method or the like to increase the particle size thereof, are face wash powder, body shampoo, powder stone candy, Used as a raw material for washing stones, face-washing foams, etc. ^ iJ, cosmetics.

As described above, powdered using a roll mill or combil type powder mill equipment, the content of particles with a particle size of 0.16 mm or less is less than 10%, and the particle size is 0.35 5 mm N-acylaminoic acid or its salt prepared in powders not containing the above particles and having a force density of 0.4 _g cm ³ or more does not feel the rough feeling when pulverized by hand. In addition, it is difficult for powdering to occur and a face washing powder can be achieved, but the composition (formulation) of the face washing powder at that time may be in accordance with conventional methods, and one or more additives may be added. Such additives can also be appropriately selected from known additives according to the desired properties.

In addition, as described above, after pulverization using a roll mill or combil type powder mill equipment, the obtained powder is fluidized by fluidized legislation to increase the particle diameter, and the average particle diameter (cumulative 50 % particle diameter) 0. 5 0 0 mm or more, 5. 0 0 0 mm below the force of density in 0. 8 g / cm ³ or less of the powder was prepared N- Ashiruamino acid or its salt Is particularly suitable as a raw material component for a face-washing foam, but the composition (formulation) of the face-washing foam at that time may be in accordance with conventional methods, and one or more additives may be combined. Such additives can be appropriately selected from known additives according to the desired properties. EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated further in detail, this invention is not limited to these Examples.

As raw materials 1 to 7, powder obtained by drying a 30% surfactant solution by fluidized granulation drying method was used.

The particle size distribution, cumulative particle size, and bulk density of the raw materials and the powdered products (products) obtained in the examples and comparative examples were measured and calculated by the following methods.

Table 1 shows the setting conditions for the powder mill, Table 2 shows the bulk density, moisture content, continuous time and evaluation of the raw material (powder before powder), and Table 3 shows the raw material (powder before powder). Table 4 shows the particle size distribution of the spread product (powdered powder), and Table 4 shows the cumulative diameter of the raw material (powder before pulverization) (20%, 30%, 40%, 50%, 85% and Table 5 shows the particle size distribution of the evaluation sample. Table 6 shows the products of Examples 3, 6, and 7 (powdered powder) and the physical property evaluation of the evaluation sample.

(1) Particle size distribution

The sieving method was used for the measurement, and classification was carried out by shaking with an automatic sieving machine made by Rctsch with an amplitude of 2.0 mm for 15 minutes. A saucer, 0.106 mm sieve, 0.150 ram sieve, 0.212 mm sieve, 0.300 mm sieve, 0.355 mm sieve, 0.500 mm sieve, 0.710 mm sieve, 0.850 mm sieve, 1.000 mm sieve, 2.360 mm sieve were used. When the weight of powder on each sieve ^{XI, X2, X 3, X4} , X5, X 6, X7, X8 and the _{_S} X9 _S X10, XI 1, expressed as a cumulative graph calculated as follows did.

0.106mm = X1 / (∑X1 ~ 1 l) X100 [%]

0.150mm = (X1 + X2) / (∑X1 ~ 11) [%]

0.212 隱 = (X1 + X2 + X3) / (∑X1 ～: L 1) [%]

(2) Cumulative particle size

Average particle size, cumulative 5% diameter, and cumulative 80% diameter! / Is obtained by linear approximation between the plots of the cumulative graph of the particle size distribution. The calculation is as shown in the following example.

Calculation example

(Assuming XI = 5, X2 = 15, X3 = 35, X4 = 25 _s X5 = 15, X6 = 5) 0. 106ram = 5 / (5 + 15 + 35 + 25 + 15 + 5) X 100 = 5%

0. 150ram = (5 + 15) / (5 + 15 + 35 + 25 + 15 + 5) X 100 = 2 0%

0.212 瞧 = (5+ 15 + 35) / (5 + 15 + 35 + 25 + 15 + 5) X 100 = 5 5%

0.300mm = (5 + 15 + 35 + 25) / (5 + 15 + 35 + 25 + 15 + 5) X 100 = 8 0%

0. 355rnm = (5+ 15 + 35 + 25 + 15) I (5 + 15 + 35 + 25 + 15 + 5) X 100 = 9 5%

0. 500mm = (5 + 15 + 35 + 25 + 15 + 5) / (5 + 15 + 35 + 25 + 15 + 5) X 100 = 1 0 0% Cumulative 95% Particle size = 0. 355+ (0 500-0.355) / (100-95) X (95-95)

Cumulative 70% particle size = 0.212+ (0. 300-0.212) / (80-55) X (70-55)

Cumulative 50% particle size = 0. 150+ (0. 212-0. 150) / (50-20) X (50-20)

Cumulative 40% particle size = 0. 150+ (0. 212—0. 150) / (55-20) X (30-20)

Cumulative 20% particle size = 0. 150+ (0. 212-0. 150) / (55-20) X (20-20)

(3) Bulk density

Use a lOOcc bulk density measuring container (5. 3ramO X 50. 3H) for bulk density, feed the powder from above 30 cm at a feed rate of about 50 _g / min so that the powder is evenly distributed from above, and cover the top surface. Grind and measure the weight (rough filling bulk density).

(4) Physical property evaluation of products (powder)

(4-1) Hand washing feeling

Evaluation of hand-washing feeling was evaluated visually by taking 0.2 g of an evaluation sample on the palm, adding 2. Og of tap water, and mixing 20 times with fingers. Observations were made by two expert panels based on the following evaluation criteria, and the average value of the two evaluation points was calculated. The evaluation criteria were 1 point or more and less than 2 points as X, 2 points or more and less than 3 points as △, 3 points or more and less than 4 points as ◯, and 4 points as ◎. The results are shown in Tables 1 to 3.

1 point: Large agglomerates remain

2 points: Somewhat undissolved

3 points: dissolves uniformly

4 points: dissolves quickly (4-2) Powder standing

For the evaluation of powder standing, evaluate the condition when a 50 g sample is dropped from a height of 50 cm.

Expertise ,. By two members, sensory evaluation was performed according to the following evaluation criteria. According to the average score of the two people, 1 or more and less than 2 points were X, 2 or more and less than 4 points were △, 4 or more points were ◯ did.

1 point

2 points

3 points

Fortune telling

5 fortune telling

(4-3) Bulk density evaluation

The transportation cost was directly evaluated by the value of bulk density. The following are the evaluation criteria. 0.3g / cc or less X

0.3-0.4g / cc Δ

0.4 ~ 0.5g / cc ○

0.5g / cc or more ◎

(5) Joint key evaluation

Even if each βΐ powdered for more than 0 minutes, no overload occurs, and when the load is constant, ○, even if it does not stop at each device overload, the adhesion amount increases after 10 minutes, and the load is reduced. △ if it has increased, X if it has stopped due to overload within 10 minutes.

Ν—Lauroureno L-Gnoretamic acid aspect ratio (long side / short side) of 2 or less powder (raw material 1) is rolled into a single gear (roll surface is gear shape) (Maximum particle size of the powder to be manufactured (target value): 0.5 mm).

The grinding conditions are as follows.

Powder feed rate: 3.2 kg / hr / cra-mall

Pitch width of gear on roll surface: 0.6 ：

Roll clearance (Distance between a pair of rolls): 0.1 1 Awakening

Roll rotation speed ratio: 1.0

Clearance between roll and scraper blade (distance between roll and scraper blade): 0, 05 mm Example 2>

A powder with an aspect ratio (long side / short side) of 2 or less of N-lauroinole-L-sodium gnoretamate as in Example 1 except that the clearance of the mouthpiece was changed to 0.19 mm. The body (raw material 1) was crushed (maximum particle size of powder to be manufactured (target value): 0.7 mm.

<Example 3> '

N-Lauroy L L-Natrium glutamate with a aspect ratio (long side / short side) of 2 or less (raw material 1) was pulverized with a two-stage gear-shaped (Rhino surface is gear-shaped) (Maximum particle size of powder to be manufactured (target value): 0.35 resolution).

The grinding conditions are as follows.

Powder feed rate: 3.2kg / hr / ctn-roll

The pitch width of the gear on the surface of the first stage mouthpiece: 0.6 mm

First stage clearance (separate distance between a pair of openings): 0. 19 mm First stage opening ¾i degree ratio: 1.0

Clearance between roll of 1st-stage roll and scraper blade (separation distance between roll and scraper blade): 0.05 mm

The pitch width of the gear on the surface of the second stage mouthpiece: 0.3 mm

2nd stage clearance (separate distance between a pair of openings): 0.23 瞧 Roll speed ratio of the second roll: 1.0

Clearance between the roll of the second-stage roll and the cutting blade (separation distance between the roll and the cutting blade): 0.05 mm Example 4>

N-Lauroyux L-Natrium glutamate having a aspect ratio (long side / short side) of 2 or less (raw material 1) was ground with a roll gear in a single gear shape (roll surface is gear shape) (Maximum particle size of the powder to be manufactured (target value): 0 · 5 瞧) ₀

The powdering conditions are as follows.

Powder feed rate: 3.2 kg / hr / cm-mouth

The pitch width of the gear on one side of the mouth of the mouth: 0.6 ram

Roll clearance (separate distance between a pair of rolls): 0.07ram

Roll rotation speed ratio: 1.0

Clearance between roll and scraper blade (distance between roll and scraper blade): 0.05 mm Example 5>

A powder (raw material 2) with an aspect ratio (long side / short side) of N-coconut oil fatty acid acylglycine sodium of 2 or less, and a two-stage gear shape (low Λ¾ surface is a gear shape) (The maximum particle size of the powder to be manufactured (target value): 0.85 mm).

The grinding conditions are as follows.

Powder feed rate: 3.2 kg / hr / cm-mouth

First stage clearance (separate distance between a pair of holes): 0.43mm First stage roll speed ratio: 1.22

The pitch width of the gear on the surface of the second stage mouthpiece: 0.6 mm

2nd stage clearance (separate distance between a pair of openings): 0.35 mm Second stage roll speed ratio: 1. 22

Clearance between the roll of the second-stage roll and the scraper blade (the distance between the roll and the scraper blade): 0.05 mm Example 6>

Powder of N-coconut oil fatty acid acylglycine sodium having a aspect ratio (long side / short side) of 2 or less (the product obtained in Example 5) in a two-stage gear shape (roll surface) Was pulverized with a roll mill with a gear shape (maximum particle size of powder to be manufactured (target value): 0.35 mm).

The powdering conditions are as follows.

Powder feed rate: 1.93 kg / hr m-mouth

First stage clearance (separate distance between a pair of openings): 0.27.

First stage mouth rotation speed ratio: 1. 22

The pitch width of the gear on the top surface of the second stage mouthpiece: 0.3 mm

2nd stage clearance (the distance between the pair of openings): 0.23mm

Second stage roll speed ratio: 1. 22

Clearance between the roll of the second stage roll and the scraper blade (the distance between the roll and the scraper blade): 0.05 mm Example 7>

Powder of N-coconut oil fatty acid acylglycine sodium having a aspect ratio (long side / short side) of 2 or less (the product obtained in Example 5) in a three-stage gear shape (roll surface Was milled with a roll mill (the maximum particle diameter of the powder to be manufactured (target value): 0.35 mm) ₀

The powdering conditions are as follows.

Powder feed rate: 1. 93 kg / hr / cm-mall The pitch width of the gear on the surface of the first stage mouthpiece: 0.6 mm

First stage clearance (separate distance between a pair of openings): 0 · 19 隱

First stage roll speed ratio: 1. 22

The pitch width of the gear on the surface of the mouth of the second stage mouthpiece: 0.6 mm

2nd stage clearance (separate distance between a pair of openings): 0.1 1 mm

Second stage mouth rotation speed ratio: 1. 22

Clearance between the roll of the second-stage roll and the scraper blade (the distance between the roll and the scraper blade): 0.05 mm

The gear pitch on the surface of the third stage mouthpiece: 0.3

3rd stage clearance (separate distance between a pair of openings): 0.15 mm

Third stage roll speed ratio: 1. 22

Clearance between the roll of the third-stage roll and the scraper blade (separation distance between the roll and the scraper blade): Example 05> 0.05 ram

N—The powder (raw material 3) with a aspect ratio (long side / short side) of coconut oil fatty acid acylglycine sodium of 2 or less is used in a two-stage gear shape (Rhino surface is a gear shape). (The maximum particle size of the powder to be manufactured (target value): 1.1 kg).

The powdering conditions are as follows.

Powder feed rate: 4. 90 kg / hr / cra-mall

The pitch width of the gear on the surface of the first stage mouth and edge: 1.0 隱

1st stage clearance (separate distance between a pair of openings): 0 · 99 瞧

First stage roll speed ratio: 1. 22

Gear pitch on the surface of the second stage mouthpiece: 1.0 ram

2nd stage clearance (separate distance between a pair of openings): 0.51 瞧 Second stage roll speed ratio: 1.2 2

Clearance between the roll of the second roll and the scraper blade (separation distance between roll and scraper blade): 0.05 mm Example 9>

A powder (raw material 4) having an aspect ratio (long side / short side) of N-coconut oil fatty acid acylglycine sodium of 2 or less was pulverized with Comil (manufactured by Parec Co., Ltd.).

The grinding conditions are as follows.

Number of rotations of rotor blade: 3 0 0 Orpm

Mesh hole diameter of mesh plate (screen): 0.6 mm

Clearance between rotor blades and mesh plate (screen) 1 隨

N-coconut oil moon succinic acid acylglycine sodium aspect ratio (long side / short side) of 2 or less powder (raw material 5) is a vertical centrifuge pin mill (Ogino Sangyo Co., Ltd.) Made). The rotation speed was 1 0 0 0 at Orpra, and the speed was 51 $. However, the adhesion due to softening was severe and the powder passage was blocked in 5 minutes and stopped due to automatic overload prevention of the equipment. Comparative Example 2>

A powder (raw material 5) having an aspect ratio (long side / short side) of N-coconut oil fatty acid acylglycine sodium of 2 or less was pulverized by a vertical centrifugal pin mill as in Comparative Example 1.

Although the speed was constant at 700 rpm, adhesion due to softening was severe and the powder passage was blocked in 7 minutes and stopped due to automatic overload prevention of β. <Comparative Example 3>

Ν—Powder (raw material 6) having a palm oil fatty acid oil acylglycine sodium aspect ratio (long side / short side) of 2 or less was pulverized with a horizontal centrifugal pin mill (manufactured by Retsch GmbH & Co.) . Although the rotation speed was 100 0 Orpm and the speed was constant, adhesion due to softening was severe, and in 5 minutes the powder passage was blocked and stopped by automatic overload prevention of β. Comparative Example 4>

Powder of N-coconut oil fatty acid acidylaricine sodium having a aspect ratio (long side / short side) of 2 or less (raw material 6) in a horizontal centrifugal screen mill (manufactured by Retsch GmbH & Co.) Crushed.

Using a mesh with a mesh hole diameter of 0.5 mm and operating at a constant speed of 100 rpm, the adhesion due to softening was severe, and the powder passage was blocked in 3 minutes to prevent automatic overload of the equipment. did. <Comparative Example 5>

Powder of N-coconut oil fatty acid acylglycine sodium with a aspect ratio (long side / short side) of 2 or less (raw material 6) was pulverized in a horizontal centrifugal screen mill as in Comparative Example 4. did.

Using a mesh with a mesh pore size of 0.2 mm, it was operated at a constant speed of 10:00 Orpm, but the adhesion due to softening was severe, and the powder passage was blocked in 2 minutes and stopped by preventing automatic overloading of β. . Comparative Example 6>

Ν—Powder (raw material 7) with the aspect ratio (long side / short side) of coconut oil fatty acid acylglycine sodium is 2 or less in the horizontal centrifuge screen mill as in Comparative Example 4. did.

A mesh with a mesh hole diameter of 0.2 mm was operated at a constant speed with 100 000 Orptn, but the adhesion due to softening was severe and the powder passage was blocked in 4 minutes to prevent automatic overload of the equipment. did.

(Evaluation sample 1)

A 30% 7 solution of N-coconut oil fatty acid sodium acylglycine was spray-dried with a spray dryer to obtain a powder having a water content of 1.2%. (Evaluation sample 2)

A 30% aqueous solution of N-coconut oil fatty acid acylglycine sodium was dried with a drum dryer to obtain a flaky powder having a water content of 0.6%.

(Sample 3 for evaluation)

A 30% aqueous solution of N-laureuil L-sodium glutamate was spray-dried with a spray dryer to obtain a powder having a water content of 1.0%.

(Evaluation sample 4)

The powder obtained in Example 7 was used as a seed material, and a 30% 7j solution of N-coconut oil fatty acid sodium acylglycine was spray-dried with a fluid granulator to obtain a powder. The powder is raw material 3.

Table 1 Gear wheel pitch width Clearance Rotation of powder in the field Cumulative particle size Speed ratio

1st 2nd 3rd 1st 2nd 3rd 20% 30% 40% 50% 85% 95%

[mmj [mm] [mm] [ram] [mm] [mm] [thigh] [nunj [o] [brittle] Lmm] thigh] [1] Example 1 0.6 0.11 0.359 0.402 0.447 0.491 0.744 0.805 1

― ―

Example 2 0.6 0.19 0.359 0.402 0.447 0.491 0.744 0.805 1

Example 3 0.6 0.3 0.19 0.23 0.359 0.402 0.447 0.491 0.744 0.805 1 Example 4 0.6 0.07 0.359 0. 02 0.447 0.491 0.744 0.805 1

-

Example 5 0.6 0.6 0.43 0.35 0.56 0.635 0.71 0.734 0.818 0.843 1.22

― ―

Example 6 0.6 0.3 0.27 0.23 0.362 0.412 0.463 0.512 0.669 0.73 1.22 Example 7 0.6 0.6 0.3 0.19 0.11 0.15 0.362 0.412 0.463 0.512 0.669 0.73 1.22 Example 8 1.0 1.0 0.99 0.51 0.717 0.75 0.783 0.816 1.351 2.1 1.22

Table 2

table

0.15 0.212 0.3 0.355 0.5 0.71 0.85 1 2.36 Purple product 50¾

LmmJ [mm] Lmm] [mm] 瞧] Lmm] [mm] Lmm] Lmm] Diameter

[%] [] [%] [¾] [%] [%] [%] [%] [% 3 [] [mm] Raw material 1 ― ― 5.4 19.2 52.1 85.8 99.3 100 ― 0.49 Raw material 2 ― ― ― ― ― 12.1 40 98.1 100 ― 0.73 Raw material 3 ― ― ― ― ― 0 17.9 60.5 80.3 98.5 0.82 Raw material 4 6.5 17.1 25.1 48.1 65.2 84.1 98.1 100 ― ― 0.31 Raw material 5 ― ― ― 15.2 48.9 96.2 100 ― ― ― 0.36 ο

Raw material 6 ~

曰 ― ― ― 5.3 25.6 48.1 74.3 99.2 100 ― 0.52 Raw material 7 ― 12.3 48.3 89.2 98.9 100 ― ― ― ― 0.22 Example 1 13.4 19.5 45.2 85.3 93.4 100 ― ― ― ― 0.22 Example 2 5.5 8.6 16.8 42.2 70.7 99.9 100 ― ― ― 0.32 Example 3 8 16.3 39.9 85.6 100 ― ― ― ― 1 0.23 Example 4 20.3 33.3 61.6 90.9 94.3 100 ― ― ― ― 0.19 Example 5 ― ― ― ― 18.6 47.4 94.2 99.9 100 ― 0.51 Example 6 5.8 15.5 45.3 76.4 100 ― ― ― ― ― 0.23 Example 7 7.5 28.1 46.3 70.5 100 ― ― ― ― ― 0.23 Example 8 ― ― ― ― 5.7 15.3 58.2 95.4 99.1 100 0.67 Example 9 4.7 13.9 30.5 48.9 61.3 99.5 100 ― ― ― 0.30 Comparative Example 1 52.3 98.9 100 ― ― ― ― ― One ― 0.10 Comparative Example 2 28.9 49.2 83.2 99.8 100 ― ― ― One ― 0.15 Comparative Example 3 13.5 40.5 55.3 70.4 85.9 99.3 100 ― ― ― 0.19 Comparative Example 4 50.1 99.3 100 ― ― ― ― One ― ― 0.11 Comparative example 5 85.2 93.1 100 ― ― ― ― ― ― ― 0.06 Comparative example 6 48.2 84.7 97.9 100 ― ― - - A 0.11

Table 4

Table 5

Table 6 Substance Hand-washing evaluation Powder standing Example 3 L ◎ O Example 6 G © 〇 Example 7 G ◎ 〇 Evaluation sample 1 G ◎ X Evaluation sample 2 GX Δ Evaluation sample 3 L ◎ X Evaluation sample 4 GX Yes From the above results, it can be seen that according to the production method of the present invention, it is possible to continuously produce a surfactant having preferable powder physical properties as a raw material component for cosmetics and the like. In particular, the powdery lauroyl glutamic acid sodium salt and the N-coconut oil fatty acid acylylricin sodium salt obtained in Examples 3, 6, and 7 have a rough feeling during hand washing. It can be seen that the powder has a powder characteristic that is suitable for a face-washing powder and is not prone to powdering.

Using the N-lauroinole L sodium monoglutamate produced in Example 3 above, a face washing powder of the following Formulation Example 1 was prepared according to a conventional method. The unit of numerical values in the formulation examples is parts by weight.

Formulation Example 1 (Face Washing Powder)

N-Lauroy L-sodium gnoretamineate 18.0

N-Myristoyl; L Monoglutamate 1 2.0 Tanorek 1 0.0 Mannitol 2 0.0 Corn Starch 3 9 8 Methylparaben 0.2 Total 1 0 0. 0 It was difficult to use, and there was no rough feeling when washing hands.

Using the N-coconut oil fatty acid acylglycine sodium produced in Example 5 above, a facial cleansing foam of the following Formulation Example 2 was prepared according to a conventional method. The unit of numerical values in the prescription examples is the weight part.

Formulation Example 2 (Fashion Foam)

N-coconut oil fatty acid sodium acylglycine 1 8 0 Glycerin 3 8 0 Coconut oil fatty acid amidpropyl betaine 1 2 Polyquaterumu 3 9 0 Lauric acid 0 4 Myristic acid 0 Stearic acid 0.4 Dariconole distearate 1. 0 Bee; ^ Nore T Reco ^ ~ Nore 0.3 Quenic acid 0.5 Water 39.1 Total 100.0 When this facial foam was actually produced, water and polyol A cleansing foam with a good shape with less dusting, good solubility and excellent workability, and no foaming. Furthermore, when this facial cleansing foam was used, it was excellent in solubility and foaming, and the usability was good.

Industrial applicability

According to the present invention, a powder suitable for washing, which has a high bulk density but does not substantially contain coarse particles, and has a small content of particles having a fine particle size that causes powdering. Powdered N-long chain acylamino acids or their salts with physical properties can be continuously produced, and powdery surface activity with suitable powder properties that has been difficult in the past Continuous mass production of chemicals at the industrial level becomes possible.

In addition, according to the present invention, there is provided a powdery N-long chain acylamino acid or a salt thereof that can give a cleansing powder that does not feel rough when hand-washed and hardly causes powdering. This application is based on Japanese Patent Application No. 2004-216536 filed in Japan, the contents of which are incorporated in full herein.

Claims

The scope of the claims

1. A process for producing powdered N-long chain acylamino acid or a salt thereof, comprising a step of pulverizing N-long chain acyl amino acid or a salt thereof with a roll mill.

2. The roll mill has one or more rolls with a gear-like surface, and the pitch width of the gears in the first roll is at least 30% particle diameter and less than 95% particle diameter of the feed powder. The method of claim 1, wherein:

3. Clearance between one and the other of each step of a single step or multiple steps is 0.12 times or more, 1 time the pitch width of the gear on the surface The method of claim 2, which is:

4. The method according to claim 2 or 3, wherein the pitch width of the gear on the roll surface of the final roll is 0.35 mm or less.

5. Roll miller, which has one or more rolls with smooth surfaces, and the clearance between one and the other of the first stage rolls is more than the cumulative 30% particle diameter of the feed powder, and the cumulative 95% particle diameter The method of claim 1, which is:

6. The rotation speed ratio of one roll and the other roll in each roll of a single roll or a multi-stage roll is 1.0 to L; The method described in the paragraph.

7. The method according to claim 5 or 6, wherein the clearance of the last stage mouthpiece is 0.35 mm or less.

8. N-long chain acyl amino acid or its salt strength S before pulverization, a powder with a bulk density of 0.4 g / cm ³ or more and a particle size of 0.16 mm or less and less than 10% The method according to any one of claims 1 to 7, which is any one of claims 1 to 7.

9. Using equipment equipped with a crushing mechanism that discharges the material supplied to the gap between the rotor blade and the mesh plate arranged on the side of the rotor blade from the mesh hole of the mesh plate, N-long chain acylamino acid or A method for producing a powdery N long-chain amino acid or salt thereof, characterized by passing through a step of grinding the salt.

10. The method according to claim 9, wherein the mesh plate has a mesh pore size of 0.25 to 2 times the cumulative 90% particle size of the field powder.

11. The method according to claim 9 or 10, wherein a clearance between the rotor blade and the mesh plate is 0.0 l to 5 mm.

12. N-long chain acyl amino acid before pulverization or its salt strength Bulk density 0.4 gcm ³ or more, particle size 0.1106 mm or less The content of particles is less than 10% The method according to any one of Items 9 to 11.

13. Crush the material supplied to the gap between the Rono Le Minole or the rotor blades and the mesh plate arranged on the side of the rotor blades with equipment equipped with a powder stone mechanism that discharges the mesh plate from the mesh holes. The method according to any one of claims 1 to 12, further comprising a step of fluidly granulating the obtained powder of N-long chain acylamino acid or a salt thereof to increase the particle diameter thereof. .

14. Powders with a particle size of less than 0.16 mm and a particle density of less than 10%, particles with a particle size of 0.3 55 mm or more and a bulk density of 0.4 gZc m ³ or more A powdered N-long chain amino acid or a salt thereof, characterized in that:

15. A facial cleansing powder comprising the powdery N-long chain acyl amino acid or a salt thereof according to claim 14.

16. A face-washing powder comprising powdery N-long chain acylamino acid or a salt thereof produced by the method according to claim 4 or 7.