JP2008056822A - Method for granulating cation-modified water-soluble polymer powder - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method by which operation efficiency during dissolving of cation-modified water-soluble polymer powder in water is improved for sufficiently preventing formation of undissolved lumps during dissolving thereof in water in the method because a cation-modified water-soluble polymer has higher hydrating properties than those of a cation-unmodified water-soluble polymer. <P>SOLUTION: The method for granulating the cation-modified water-soluble polymer is carried out as follows. Water or an aqueous solution of the cation-modified water-soluble polymer as a binder is added to the cation-modified water-soluble polymer and hydration and granulation are then conducted until the moisture in the cation-modified water-soluble polymer becomes the range of 1-13 mass%. Furthermore, the granulation is then carried out with a dry compression granulator. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  In the present invention, water or a cation-modified water-soluble polymer aqueous solution is added as a binder to a cation-modified water-soluble polymer, and after water granulation until the water content is in the range of 1 to 13% by mass, dry compression molding is further performed. It relates to a method of granulating a cation-modified water-soluble polymer, characterized by granulating with a granulator, and suppresses the generation of spatter when dissolved in water without using any solubility improver, and The present invention relates to a method for granulating a cation-modified water-soluble polymer that can improve workability without requiring time for dissolution.

  In general, cellulose, polysaccharides and their derivatives as water-soluble polymer compounds are poorly dispersible in water, so that they easily become a powder (Mamako) when thrown into water. However, there is a disadvantage that it must be added little by little. Conventionally, as a method of improving this defect, a method of granulating by adding a binder to a water-soluble polymer compound has been proposed.

  Patent Document 1 discloses a method for producing a water-soluble polysaccharide as a method for producing a water-soluble polysaccharide having excellent workability such as solubility in water, suppression of foaming at the time of dissolution, and suppression of powdering at the time of handling. A method for producing a water-soluble polysaccharide, characterized in that a water-soluble polysaccharide and an emulsifier such as tetraglycerin monooleate are used as the binder liquid by granulating while spraying the binder liquid onto the powder of the water-soluble polysaccharide. Are listed.

  In Patent Document 2, as a liquid food thickening food thickener and a method for producing the same, granulation is performed without reducing the swelling / dissolving / thickening effect of the thickening polysaccharide as much as possible. As a method for providing a granular liquid food thickener capable of exhibiting stabilized thickening, a granular thickening polysaccharide obtained by treating a powdered thickening polysaccharide using a modified starch aqueous solution as a binder There is described a liquid food thickener and a liquid food thickener production method for granulating a powdered thickening polysaccharide in a fluidized bed granulating apparatus or a similar apparatus.

  Patent Document 3 discloses a pharmaceutical composition with improved solubility and fluidity, which can be applied to a wider range of poorly water-soluble drugs and has improved poorly water-soluble drug solubility and fluidity obtained by a simple production method. As a pharmaceutical composition, a pharmaceutical composition containing a granulated product obtained by granulating a mixture of a poorly water-soluble drug and a fluidizing agent with water or a hydrous alcohol solution of a water-soluble polymer is described. ing.

  In Patent Document 4, as a granulated coated seed and a method for producing the same, a seed, particularly a phobic seed, which is granulated and coated, is easy to absorb water at the time of sowing, more easily broken by water absorption, and the cracking changes with time. In order to provide a granulated coated seed which is difficult to be formed and has almost no by-product of a spherical substance containing no seed, a powder having a mean particle size of 30 μm or less and montmorillonite and bentonite composed of one or both of montmorillonite and bentonite A granulated composition containing a granulated material comprising a powder having an average particle size of 10 μm or more and 30 μm or less, and a cellulose-based water solution having an aqueous solution viscosity at 25 ° C. of 50 mPa · s or less as a binder Describes a method for producing a granulated coating of seeds using an aqueous solution of a functional polymer.

However, when a cation-modified water-soluble polymer compound whose solubility is adjusted by the method described in the above-mentioned prior art document is blended in cosmetics or the like, there is a problem that undesirable components cannot be mixed. In addition, the cation-modified water-soluble polymer has higher hydration property than the water-soluble polymer that is not cation-modified, and the above method cannot sufficiently prevent the generation of a spatter when dissolved in water. Further, depending on the granulation method, there is a problem that it takes time to dissolve even if the occurrence of mamako can be suppressed.
JP 2000-63402 A (page 1-5) JP 2004-147567 A (page 1-8) JP 2005-82503 A (page 1-5) JP 10-225207 A (page 1-6)

  An object of the present invention is to solve the above-described problems of the prior art and to provide a method for effectively improving the workability at the time of dissolving the cation-modified water-soluble polymer powder in water.

  As a result of intensive studies to solve the above problems, the present inventors have found that water or a cation-modified water-soluble polymer aqueous solution is added to a powder of a cation-modified water-soluble polymer such as cellulose or a cation-modified derivative of a polysaccharide. Is added as a binder, and the mixture is hydro-granulated until the moisture content of the powder is in the range of 1 to 13% by mass, and further granulated with a dry compression granulator, so that a solubility improver is used at all. The present inventors have found that it is possible to prevent generation of a spatter at the time of dissolution in water and that the dissolution time does not require time, and the present invention has been completed.

  That is, in the present invention, water or a cation-modified water-soluble polymer aqueous solution is added as a binder to the cation-modified water-soluble polymer, and the mixture is granulated until the water content of the cation-modified water-soluble polymer is in the range of 1 to 13% by mass. Then, it is related with the granulation method of the cation modified | denatured water-soluble polymer characterized by further granulating with a dry compression granulator.

  Water or a cation-modified water-soluble polymer aqueous solution is added as a binder, water is granulated to a moisture content of 1 to 13% by mass, and then granulated with a dry compression granulator to obtain water. It is possible to improve the workability at the time of dissolving the cation-modified water-soluble polymer compound in water without generating spatter during dissolution in water and without requiring time for dissolution.

The present invention will be described in detail below.
Examples of the cation-modified water-soluble polymer to be subjected to hydrogranulation include cation-modified derivatives of cellulose or polysaccharide. Examples of cellulose derivatives include cation-modified cellulose, cation-modified hydroxyethyl cellulose, and polysaccharides and derivatives thereof include guar gum, locust bean gum, fenugreek gum, tara gum, tamarind gum, psyllium seed gum, quinseed gum, carrageenan, Alginate, agar, taracan gum, gum arabic, karaya gum, starch, hydroxyethyl guar gum, hydroxyethyl starch, methyl guar gum, methyl starch, ethyl guar gum, hydroxypropyl guar gum, hydroxypropyl starch, hydroxyethyl methyl guar gum, hydroxyethyl methyl starch, Hydroxypropyl methyl guar gum, acetylated or alkylated starch, hydroxypropyl methyl star , Dextrin, cationic-modified derivatives such as dextran can be exemplified.

(式中Ｒ_１、Ｒ_２は各々炭素数１〜３個のアルキル基、Ｒ_３は炭素数１〜２４のアルキル基を示し、Ｘ⁻は陰イオンを示す。nは、ｎ＝０又はｎ＝１〜３０を示し、ｎ＝１〜３０の時、（Ｒ_４Ｏ）_nは炭素数２〜４のアルキレンオキサイドの重合体残基であって、単一のアルキレンオキサイドからなるポリアルキレングリコール鎖及び／又は２種類以上のアルキレンオキサイドからなるポリアルキレングリコール鎖を示す。) The method of cation modification is not particularly limited, and examples thereof include a method of reacting an arbitrary quaternary ammonium salt with a water-soluble polymer. Specifically, for example, unmodified fenugreek gum, tara gum, locust bean It can be obtained by replacing part of the hydroxyl groups of gum and hydroxyethyl cellulose with a quaternary nitrogen-containing group represented by the following chemical formula (1).

(Wherein R ₁ and R ₂ are each an alkyl group having 1 to ₃ carbon atoms, R ₃ is an alkyl group having 1 to 24 carbon atoms, X ⁻ is an anion, and n is n = 0 or n = 1-30, and when n = 1-30, (R ₄ O) _n is a polymer residue of alkylene oxide having 2 to 4 carbon atoms, and is a polyalkylene glycol chain consisting of a single alkylene oxide And / or a polyalkylene glycol chain composed of two or more alkylene oxides.)

  In the present invention, water or an aqueous solution of a cation-modified water-soluble polymer is used as the binder. Examples of water include tap water, distilled water, purified water, and ion exchange water. Moreover, what contained water-soluble solvents, such as alcohol, and inorganic salt in the range which does not impair the objective of this invention may be used. Examples of the cation-modified water-soluble polymer aqueous solution include the aqueous solution of the cation-modified water-soluble polymer described above. Here, the aqueous solution may be an aqueous solution of a cation-modified water-soluble polymer to be granulated or an aqueous solution of a cation-modified water-soluble polymer that is not to be granulated.

  As a device used for hydro-granulation, a device equipped with a spray nozzle capable of spraying a liquid to a fluidized powder and granulating a powder is excellent in disintegration, fluidity and water solubility. It is preferable in that excellent porous granulated particles can be produced. Specifically, a fluidized bed granulation coating apparatus “Flow Coater” manufactured by Freund Sangyo Co., Ltd., a “Glatt fluidized bed processor” manufactured by Glatt Co., Ltd. sold by POWREC, Inc. and the like can be preferably used. In addition, a high-speed agitation granulator / dryer “Microwave Granulator / Dryer” manufactured by Fukae Pautech Co., Ltd. can be used as the hydro-granulator.

  The present invention is characterized in that it is granulated with a dry compression granulator after the water content of the powder is hydrated to a range of 1 to 13% by mass. When the water content of the powder granulated by the dry compression granulator exceeds 13%, the granulated powder becomes hard, and the core-shaped splint remains, and when dissolved in water. Hydration time and dissolution time become too long, resulting in energy loss. Particularly preferably, the moisture content of the powder granulated by the dry compression granulator is 5 to 12% by mass, and the hydration time of the granulated powder granulated by the dry compression granulator is in an appropriate range. Inside, no generation of spatter when dissolved in water is observed and much time is not required for dissolution. In addition, there is an advantage that the amount of particles of 250 μm pass is reduced and the amount returned to the hydro-granulator can be reduced.

  As the dry compression granulator, a type of apparatus that can be equipped with a compression roll and a screw and can freely adjust the compression force of the hydraulic cylinder can be preferably used. Specifically, Freund Sangyo Co., Ltd. dry granulator “Roller Compactor”, Kurimoto Steel Works dry compression granulation system “Roller Compactor”, Turbo Kogyo Co., Ltd. roll compression granulator “Roller Compactor” "A dry granulator" Alexander Roller Compactor "sold by Matsubo Co., Ltd. can be used.

  Examples of the present invention will be described below in comparison with comparative examples, but the present invention is not particularly limited to these examples. In the following Examples and Comparative Examples, cation-modified hydroxyethyl cellulose (polyquaternium-10) to which no solubility improver was added was used as the cation-modified water-soluble polymer compound. After adding a certain amount of water or a cation-modified hydroxyethylcellulose 2.0% aqueous solution to this with a spray nozzle, granulate with a fluidized bed granulator at a hot air temperature of 60-80 ° C. until the water content becomes 1-13 mass%. The dried powder was taken out, and then the granulated product having a constant particle size was obtained through a crusher and a granulator with respect to the powder granulated by a dry compression granulator. For each sample having different moisture content, the amount of the sample was adjusted and adjusted to be a 2% aqueous solution in terms of solid content, and used for evaluation.

[Example 1]
Purified water (5.0 kg) was added to cation-modified hydroxyethyl cellulose powder (10 kg) at an addition rate of 167 g / min, and granulated and dried while gradually raising the hot air temperature to 60 to 80 ° C. Air flow rate was increased to 8.0m ³ / min to 9.5m ³ / minute. As a fluidized granulation drying apparatus, a fluidized bed granulation coating apparatus “Flow Coater” FLO-30SJ type manufactured by Freund Corporation was used. Moisture was measured during granulation drying, and the powder whose water content became 10% by mass was subjected to Freund Sangyo Co., Ltd. dry granulator “Roller Compactor Tabletop Type TF-Labo” and granulator (1000 μm screen used). Used and dry granulated. Granulation conditions are: Roll type: S type Screw type: B type Gap between rollers: 0.35 mm
Screw rotation speed: 15-20rpm
Roll pressure: 12Mpa
This sample was designated as Product 1 of the present invention.

[Example 2]
A fluidized bed granulation coating apparatus “Flow Coater” FLO-30SJ type was used under the same conditions as in Example 1 and the moisture content during granulation drying was measured. Dry granulation was performed using a dry granulator “Roller Compactor Desktop Type TF-Labo” and a granulator (using a 1000 μm screen). This sample was designated as Product 2 of the present invention.

Example 3
A fluidized bed granulation coating apparatus “Flow Coater” FLO-30SJ type was used under the same conditions as in Example 1, and the water content during granulation drying was measured. Dry granulation was performed using a dry granulator “Roller Compactor Desktop Type TF-Labo” and a granulator (using a 1000 μm screen). This sample was designated as Product 3 of the present invention.

Example 4
To 10 kg of the cation-modified hydroxyethylcellulose powder, 1.67 kg of a 2% aqueous solution of cation-modified hydroxyethylcellulose was added at an addition rate of 278 g / min, and granulated and dried while gradually raising the hot air temperature to 60 to 80 ° C. Air flow rate was increased to 8m ³ / min to 15m ³ / min. As a fluidized granulating and drying apparatus, a “Glatt fluidized bed processor” WSG30 type manufactured by Glatt Co., Ltd., sold by POWREC, Inc. was used. Moisture was measured during granulation and drying, and the powder with a moisture content of 7% by mass was subjected to Freund Sangyo Co., Ltd. dry granulator “Roller Compactor Desktop TF-Labo” and granulator (1000 μm screen used). Used and dry granulated. This sample was designated as Product 4 of the present invention.

[Comparative Example 1]
0.8 kg of purified water was added to 10 kg of cation-modified hydroxyethyl cellulose powder at an addition rate of 167 g / min, and a batch type hydrolyzer “Vertical Granulator” sold by POWREC was used. This hydrolyzed powder (water content 8% by mass) was dry granulated using a dry granulator “Roller Compactor Desktop Type TF-Labo” manufactured by Freund Sangyo Co., Ltd. and a granulator (using a 1000 μm screen). This sample was designated as comparative product 1.

[Comparative Example 2]
Purified water (5.0 kg) was added to cation-modified hydroxyethyl cellulose powder (10 kg) at an addition rate of 167 g / min, and granulated and dried while gradually raising the hot air temperature to 60 to 80 ° C. Air flow rate was increased to 8.0m ³ / min to 9.5m ³ / minute. As a fluidized granulation drying apparatus, a fluidized bed granulation coating apparatus “Flow Coater” FLO-30SJ type manufactured by Freund Corporation was used. During the granulation drying, the moisture content was measured and the powder whose moisture content was 13.5% by mass was used as a dry granulator “Roller Compactor Desktop Type TF-Labo” manufactured by Freund Sangyo Co., Ltd. and a granulator (1000 μm screen used) ) Was used for dry granulation. This sample was designated as comparative product 2.

[Comparative Example 3]
The cation-modified hydroxyethyl cellulose (product with no solubility improver added) powder used in Examples 1 to 4 was used as Comparative Product 3.

[Comparative Example 4]
In the drying step when obtaining the cation-modified hydroxyethyl cellulose powder, the drying is stopped when the water content becomes 12% by mass, and the water-containing cation-modified cellulose powder is produced by Freund Sangyo Co., Ltd. dry granulator. Dry granulation was performed using a “Roller Compactor Desktop TF-Labo” and a granulator (using a 1000 μm screen). This sample was designated as comparative product 4.

〔Evaluation methods〕
For each sample with different moisture content, the amount of the sample is adjusted so that it becomes a 2% aqueous solution in terms of solid content, and the sample is poured into 20 ° C. water that is being stirred at once to hydrate and the viscosity rapidly increases. The time until the viscosity increased after the addition was confirmed by visual observation and measured as the hydration time. At the same time, the presence or absence of generation of spatter at the time of charging was confirmed. Furthermore, stirring was continued in the aqueous solution after measurement of the hydration time, and the time from the time of charging until the time when the spatter and the core spatter were dissolved to form a uniform aqueous solution was measured as the dissolution time. In addition, the water | moisture content was measured on 105 degreeC and the conditions for 30 minutes using the infrared moisture meter FD-600 by a KETT scientific research company company.

〔Evaluation results〕
Table 1 shows the results of measurement of the hydration time and presence / absence of occurrence of pollination of the inventive products 1 to 4 and the comparative products 1 to 3.

  From the above evaluation results, water or a cation-modified water-soluble polymer aqueous solution is used as a binder for the cation-modified water-soluble polymer, granulated by a hydro-granulator, and the water content of the powder is in the range of 1 to 13% by mass. In the case of the powder granulated with a dry compression granulator after being granulated until it was, it was confirmed that it was difficult to form a joint powder when dissolved in water. By the method of the present invention, it is possible to suppress generation of a spatter during dissolution in water without using a solubility improver and improve solubility such as dissolution time. A cosmetic composition containing the cation-modified water-soluble polymer compound produced by this method can be provided.

Example 6
Table 2 shows specific shampoo formulations of cosmetic compositions containing the cation-modified water-soluble polymer compound produced by the method of the present invention.

Claims (3)

Water or a cation-modified water-soluble polymer aqueous solution is added as a binder to the cation-modified water-soluble polymer, and after water granulation until the water content is in the range of 1 to 13% by mass, further granulation is performed with a dry compression granulator. A method for granulating a cation-modified water-soluble polymer. The method for granulating a cation-modified water-soluble polymer according to claim 1, wherein the cation-modified water-soluble polymer is a cation-modified derivative of cellulose or polysaccharide. A cosmetic composition comprising a cation-modified water-soluble polymer granulated by the method according to claim 1 or 2.