JP7370178B2 - Method for manufacturing dentifrice granules - Google Patents
Method for manufacturing dentifrice granules Download PDFInfo
- Publication number
- JP7370178B2 JP7370178B2 JP2019117568A JP2019117568A JP7370178B2 JP 7370178 B2 JP7370178 B2 JP 7370178B2 JP 2019117568 A JP2019117568 A JP 2019117568A JP 2019117568 A JP2019117568 A JP 2019117568A JP 7370178 B2 JP7370178 B2 JP 7370178B2
- Authority
- JP
- Japan
- Prior art keywords
- water
- organic binder
- granules
- powder material
- insoluble powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000008187 granular material Substances 0.000 title claims description 123
- 239000000551 dentifrice Substances 0.000 title claims description 85
- 238000004519 manufacturing process Methods 0.000 title claims description 41
- 238000000034 method Methods 0.000 title claims description 26
- 239000011230 binding agent Substances 0.000 claims description 102
- 239000000843 powder Substances 0.000 claims description 76
- 239000000463 material Substances 0.000 claims description 73
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- 239000011148 porous material Substances 0.000 claims description 34
- 238000002844 melting Methods 0.000 claims description 33
- 230000008018 melting Effects 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 29
- 239000002562 thickening agent Substances 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 239000001993 wax Substances 0.000 claims description 17
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 16
- 239000000194 fatty acid Substances 0.000 claims description 16
- 229930195729 fatty acid Natural products 0.000 claims description 16
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 9
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
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Description
本発明は、歯磨剤用顆粒の製造方法に関する。 The present invention relates to a method for manufacturing dentifrice granules.
近年、虫歯や歯周病の原因となる歯垢を効率よく除去し、触知できるような顆粒を配合した歯磨剤が知られている。
例えば、特許文献１には、水不溶性粉末材料と珪酸塩とを容器回転型造粒機を用いて混合し、顆粒化する歯磨剤用顆粒の製造方法であって、多流体ノズルを用いて、該水不溶性粉末材料に該珪酸塩の水溶液を液滴として供給し、造粒する工程を含む、歯磨剤用顆粒の製造方法が開示されている。
In recent years, dentifrices containing palpable granules that efficiently remove dental plaque, which causes cavities and periodontal disease, have become known.
For example, Patent Document 1 discloses a method for producing dentifrice granules in which a water-insoluble powder material and a silicate are mixed using a container rotary granulator and granulated, using a multifluid nozzle. A method for producing dentifrice granules is disclosed, which includes a step of supplying an aqueous solution of the silicate as droplets to the water-insoluble powder material and granulating it.
従来、歯磨剤用顆粒の結合剤としては、各種の水溶性結合剤や水不溶性結合剤が使われてきた。特許文献１のように珪酸塩の水溶液を用いた場合は、乾燥工程に時間とコストがかかるため、生産性が低いという課題がある。
本発明は、適度な細孔容積を有し、歯磨剤用として好適な顆粒を効率よく製造する方法に関する。
Conventionally, various water-soluble binders and water-insoluble binders have been used as binders for dentifrice granules. When an aqueous solution of silicate is used as in Patent Document 1, the drying process takes time and cost, so there is a problem that productivity is low.
The present invention relates to a method for efficiently producing granules having a suitable pore volume and suitable for use in dentifrice.
本発明者らは、水不溶性粉末材料と融点以上の温度に加熱した有機結合剤とを、容器回転型混合機と多流体ノズルとを用いて顆粒化することにより、歯磨剤用顆粒を効率よく製造しうることを見出した。
すなわち、本発明は、次の〔１〕～〔３〕に関する。
〔１〕 水不溶性粉末材料及び融点以上の温度に加熱した有機結合剤を、容器回転型混合機を用いて混合する工程を有し、該有機結合剤の融点が２５℃以上であり、該工程において、多流体ノズルを用いて、水不溶性粉末材料に有機結合剤を供給する、歯磨剤用顆粒の製造方法。
〔２〕前記〔１〕の方法で得られる歯磨剤用顆粒。
〔３〕有機結合剤と水不溶性粉末材料とを含有する歯磨剤用顆粒であって、水不溶性粉末材料の含有量が３０～９５質量％であり、有機結合剤の含有量が５～７０質量％であり、直径０．１～１０μｍの細孔の容積（以下、「０．１～１０μｍの細孔の容積」を、単に「細孔容積」ともいう）が０．０７～１ｍＬ／ｇである、歯磨剤用顆粒。
The present inventors have efficiently produced dentifrice granules by granulating a water-insoluble powder material and an organic binder heated to a temperature above the melting point using a container rotating mixer and a multifluid nozzle. We discovered that it can be manufactured.
That is, the present invention relates to the following [1] to [3].
[1] A step of mixing a water-insoluble powder material and an organic binder heated to a temperature higher than the melting point using a container rotating mixer, the melting point of the organic binder is 25° C. or higher, and the step A method for producing dentifrice granules, comprising supplying an organic binder to a water-insoluble powder material using a multifluid nozzle.
[2] Granules for dentifrice obtained by the method of [1] above.
[3] Granules for dentifrice containing an organic binder and a water-insoluble powder material, in which the content of the water-insoluble powder material is 30 to 95% by mass, and the content of the organic binder is 5 to 70% by mass %, and the volume of pores with a diameter of 0.1 to 10 μm (hereinafter, "volume of pores with a diameter of 0.1 to 10 μm" is also simply referred to as "pore volume") is 0.07 to 1 mL/g. There are granules for toothpaste.
本発明の歯磨剤用顆粒の製造方法によれば、適度な細孔容積を有し、歯磨剤用として好適な顆粒を効率よく製造する方法を提供することができる。 According to the method for producing granules for dentifrice of the present invention, it is possible to provide a method for efficiently producing granules having an appropriate pore volume and suitable for use in dentifrice.
［歯磨剤用顆粒の製造方法］
本発明の歯磨剤用顆粒の製造方法は、水不溶性粉末材料及び融点以上の温度に加熱した有機結合剤を、容器回転型混合機を用いて混合する工程を有し、該有機結合剤の融点が２５℃以上であり、該工程において、多流体ノズルを用いて、水不溶性粉末材料に有機結合剤を供給する。
本発明の歯磨剤用顆粒の製造方法によれば、従来の珪酸塩水溶液に代表される水溶性結合剤を使用した製造方法に比して、効率的に歯磨剤用顆粒を製造することができる。更に、該製造方法を採用することにより、得られる歯磨剤用顆粒が適度な細孔容積を有し、歯磨剤用として好適であり、該歯磨剤用顆粒を配合した歯磨剤の歯垢除去性能の向上にも寄与するものと考えられる。
その詳細な機構は不明であるが、一部は以下のように推定される。
容器回転型混合機を用いた顆粒化方法では、粒子を均一に流動せしめることが可能であり、更に、回転による粒子の持ち上げ及び自重による滑り・落下を伴う混合機構により、粒子に加えられるせん断力が抑制される。そのため、容器回転型混合機を用いた顆粒化方法は、非圧密な顆粒化方法ということができる。従って、容器回転型混合機を用いて得られた歯磨剤用顆粒は、適度な崩壊強度を有し、顆粒感に優れると共に、多段階で崩壊するため、ブラッシングにより多様な粒度の粒子に崩壊する。崩壊した多様な粒度の粒子が歯面に接触して効率的にブラッシング力を伝達することで、歯垢除去性能が向上すると考えられる。
また、結合剤として、融点以上の温度に加熱した有機結合剤を使用することにより、結合剤として珪酸塩水溶液に代表される水溶性結合剤等を使用した場合に比して、乾燥工程を短縮、又は乾燥工程を省略することが可能となり、効率的に歯磨剤用顆粒を製造することが可能である。更に、融点以上の温度に加熱した有機結合剤を使用することで、結合剤の水不溶性粉末材料への吸収が抑制され、高空隙、高崩壊性の歯磨剤用顆粒が得られると考えられる。これにより、上述した歯垢除去性能の向上にも寄与し得ると期待される。
以下、本発明方法に用いられる各成分、製造方法について順次説明する。
[Method for manufacturing dentifrice granules]
The method for producing dentifrice granules of the present invention includes the step of mixing a water-insoluble powder material and an organic binder heated to a temperature higher than the melting point using a container rotating mixer, the melting point of the organic binder being is at least 25° C., and in the process a multifluid nozzle is used to supply the organic binder to the water-insoluble powder material.
According to the method for producing dentifrice granules of the present invention, dentifrice granules can be produced more efficiently than conventional production methods using water-soluble binders such as silicate aqueous solutions. . Furthermore, by adopting this production method, the obtained dentifrice granules have a suitable pore volume and are suitable for use in dentifrices, and the plaque removal performance of dentifrices containing the dentifrice granules is improved. It is thought that this will also contribute to the improvement of
Although the detailed mechanism is unknown, some of the mechanisms are presumed as follows.
The granulation method using a container-rotating mixer allows the particles to flow uniformly, and furthermore, the mixing mechanism, which involves lifting the particles by rotation and sliding/falling them due to their own weight, reduces the shear force applied to the particles. is suppressed. Therefore, the granulation method using a container rotary mixer can be said to be a non-consolidated granulation method. Therefore, the dentifrice granules obtained using a container-rotating mixer have appropriate disintegration strength, excellent granularity, and disintegrate in multiple stages, so they disintegrate into particles of various sizes when brushed. . It is thought that plaque removal performance is improved by the disintegrated particles of various sizes coming into contact with the tooth surface and efficiently transmitting brushing force.
In addition, by using an organic binder heated to a temperature above its melting point as a binder, the drying process is shortened compared to when a water-soluble binder such as a silicate aqueous solution is used as a binder. Alternatively, it becomes possible to omit the drying step, and it is possible to efficiently produce dentifrice granules. Furthermore, by using an organic binder heated to a temperature above the melting point, absorption of the binder into the water-insoluble powder material is suppressed, and it is thought that dentifrice granules with high voids and high disintegration can be obtained. This is expected to contribute to the improvement in the plaque removal performance described above.
Each component and manufacturing method used in the method of the present invention will be sequentially explained below.
（水不溶性粉末材料）
本発明の方法に用いられる水不溶性粉末材料としては、歯の研磨剤に通常用いられるものが好ましく、具体的には無機材料が好ましい。ここで、「水不溶性」とは、水１００ｇに対する溶解量（２０℃）が１ｇ以下であることを意味する。
水不溶性粉末材料の具体例としては、軽質炭酸カルシウム、重質炭酸カルシウム、ゼオライト、酸化亜鉛、シリカ、第二リン酸カルシウム、第三リン酸カルシウム、不溶性メタリン酸ナトリウム、水酸化アルミニウム、リン酸マグネシウム、ピロリン酸カルシウム、炭酸マグネシウム、及び酸化チタン等から選ばれる１種以上が挙げられる。これらは単独で、又は２種以上を組み合わせて用いることができる。
これらの中でも、顆粒化した際の物性やコストの観点から、水不溶性粉末材料としては、軽質炭酸カルシウム、重質炭酸カルシウム、ゼオライト、酸化亜鉛、及びシリカから選ばれる１種以上を含むことが好ましく、フッ素化合物と安定に共存することができる観点から、シリカを含むことがより好ましい。なお、シリカやゼオライトは、通常、多孔質であるため、結合剤を吸収しやすく、その結果、歯磨剤用顆粒として好適な粒子径が得られるように顆粒化を行うために多量の結合剤を必要とする。そのため、結合剤として珪酸塩水溶液を用いた場合は、持ち込まれる水量が多く、特に、乾燥工程に時間を要するという課題がある。従って、本発明の製造方法は、特に水不溶性粉末材料としてシリカやゼオライトを使用した際に好適である。更に、本発明の製造方法は、歯磨剤用顆粒としての安全性の観点から、水不溶性粉末材料として、シリカを使用した際に特に好適に用いられる。
(Water-insoluble powder material)
As the water-insoluble powder material used in the method of the present invention, those commonly used in tooth polishing agents are preferred, and specifically inorganic materials are preferred. Here, "water-insoluble" means that the amount dissolved in 100 g of water (at 20° C.) is 1 g or less.
Specific examples of water-insoluble powder materials include light calcium carbonate, heavy calcium carbonate, zeolite, zinc oxide, silica, dibasic calcium phosphate, tribasic calcium phosphate, insoluble sodium metaphosphate, aluminum hydroxide, magnesium phosphate, calcium pyrophosphate, One or more types selected from magnesium carbonate, titanium oxide, etc. can be mentioned. These can be used alone or in combination of two or more.
Among these, from the viewpoint of physical properties and cost when granulated, the water-insoluble powder material preferably contains one or more selected from light calcium carbonate, heavy calcium carbonate, zeolite, zinc oxide, and silica. From the viewpoint of being able to coexist stably with a fluorine compound, it is more preferable that silica is included. Furthermore, since silica and zeolite are usually porous, they easily absorb binders, and as a result, a large amount of binder is added to granulate them to obtain a particle size suitable for dentifrice granules. I need. Therefore, when a silicate aqueous solution is used as a binder, there is a problem that a large amount of water is brought in, and in particular, the drying process requires time. Therefore, the production method of the present invention is particularly suitable when silica or zeolite is used as the water-insoluble powder material. Furthermore, the production method of the present invention is particularly preferably used when silica is used as the water-insoluble powder material from the viewpoint of safety as dentifrice granules.
水不溶性粉末材料の平均粒子径は、顆粒崩壊後の歯の汚れ除去の観点から、好ましくは０．１μｍ以上、より好ましくは０．５μｍ以上、更に好ましくは１μｍ以上であり、異物感を減らす観点から、その上限は、好ましくは２０μｍ以下、より好ましくは１５μｍ以下、更に好ましくは１０μｍ以下である。水不溶性粉末材料の平均粒子径は、好ましくは０．１～２０μｍ、より好ましくは０．５～１５μｍ、更に好ましくは１～１０μｍである。
平均粒子径は、実施例記載の方法により測定することができる。
The average particle diameter of the water-insoluble powder material is preferably 0.1 μm or more, more preferably 0.5 μm or more, and still more preferably 1 μm or more, from the viewpoint of removing tooth stains after granule disintegration, and from the viewpoint of reducing foreign body sensation. Therefore, the upper limit thereof is preferably 20 μm or less, more preferably 15 μm or less, and even more preferably 10 μm or less. The average particle size of the water-insoluble powder material is preferably 0.1 to 20 μm, more preferably 0.5 to 15 μm, and still more preferably 1 to 10 μm.
The average particle diameter can be measured by the method described in Examples.
（有機結合剤）
本発明において、有機結合剤は、水不溶性粉末材料を適度な細孔容積を有する顆粒に顆粒化するために用いられる。
有機結合剤は、水不溶性粉末材料を適度な細孔容積を有する顆粒に顆粒化する観点から、その融点が２５℃以上、好ましくは３０℃以上、より好ましくは４０℃以上、更に好ましくは５０℃以上であり、ノズルからの吐出性や製造中の熱負荷の観点から、好ましくは１５０℃以下、より好ましくは１００℃以下、更に好ましくは９５℃以下、更に好ましくは９０℃以下である。
有機結合剤の融点は、実施例に記載の方法により測定される。
(Organic binder)
In the present invention, organic binders are used to granulate water-insoluble powder materials into granules with moderate pore volume.
The organic binder has a melting point of 25°C or higher, preferably 30°C or higher, more preferably 40°C or higher, and even more preferably 50°C, from the viewpoint of granulating the water-insoluble powder material into granules with appropriate pore volume. From the viewpoint of ejection properties from the nozzle and heat load during production, the temperature is preferably 150°C or lower, more preferably 100°C or lower, still more preferably 95°C or lower, and still more preferably 90°C or lower.
The melting point of the organic binder is measured by the method described in the Examples.
有機結合剤としては、油脂、ワックス、高級脂肪酸又はその塩、高級アルコール、エーテル化合物等が例示される。これらの中でも、有機結合剤は、歯磨剤に配合しうる材料や入手性の観点から、油脂、ワックス、高級脂肪酸、及び高級アルコールから選ばれる１種以上を含むことが好ましく、油脂、ワックス、高級脂肪酸、及び高級アルコールから選ばれる１種以上からなることがより好ましい。
有機結合剤の分子量は、水不溶性粉末材料を適度な細孔容積を有する顆粒に顆粒化する観点から、好ましくは１００以上であり、そして、ノズルからの吐出性や製造中の熱負荷の観点から、好ましくは１，０００以下である。
有機結合剤は、水不溶性粉末材料の結合剤として用いる観点から、疎水性であることが好ましい。疎水性であるとは、２５℃において、水１００ｇに対する溶解量が１ｇ以下であることを意味する。
Examples of the organic binder include oils and fats, waxes, higher fatty acids or salts thereof, higher alcohols, and ether compounds. Among these, the organic binder preferably contains one or more selected from oils and fats, waxes, higher fatty acids, and higher alcohols, from the viewpoint of materials that can be blended into dentifrices and availability. More preferably, it is composed of one or more selected from fatty acids and higher alcohols.
The molecular weight of the organic binder is preferably 100 or more from the viewpoint of granulating the water-insoluble powder material into granules having an appropriate pore volume, and from the viewpoint of ejectability from a nozzle and heat load during manufacturing. , preferably 1,000 or less.
The organic binder is preferably hydrophobic from the viewpoint of use as a binder for water-insoluble powder materials. Being hydrophobic means that the amount dissolved in 100 g of water is 1 g or less at 25°C.
油脂としては、硬化ナタネ油、硬化ヒマシ油等の植物脂、動物脂が挙げられる。
ワックスとしては、カルナバワックス、キャンデリラワックス、ライスワックス等の植物由来のワックス、蜜ろう、鯨ろう等の天然由来のワックス；ポリプロピレンワックス、ポリエチレンワックス、ポリプロピレンポリエチレン共重合体、マイクロクリスタリンワックス、パラフィンワックス、フィッシャートロプシュワックス、サゾールワックス等の脂肪族炭化水素系ワックス、脂肪酸と高級アルコールとのエステル系ワックス、ジステアリルケトン等のケトン系ワックス等の合成ワックスが挙げられる。
高級脂肪酸としては、例えば、ラウリン酸、ミリスチン酸、ペンタデシル酸、パルミチン酸、パルミトレイン酸、ステアリン酸等の炭素数１２～３０の脂肪酸が挙げられ、ミリスチン酸、ペンタデシル酸、パルミチン酸、ステアリン酸が好ましい。
高級アルコールとしては、ミリスチルアルコール、セチルアルコール（別名：セタノール）、ステアリルアルコール、ベヘニルアルコール等の炭素数１２～３０のアルコールが挙げられる。
Examples of the fats and oils include vegetable fats such as hydrogenated rapeseed oil and hydrogenated castor oil, and animal fats.
Waxes include plant-based waxes such as carnauba wax, candelilla wax, and rice wax; natural waxes such as beeswax and spermaceti; polypropylene wax, polyethylene wax, polypropylene-polyethylene copolymer, microcrystalline wax, and paraffin wax. , aliphatic hydrocarbon waxes such as Fischer-Tropsch wax and Sasol wax, ester waxes of fatty acids and higher alcohols, and synthetic waxes such as ketone waxes such as distearyl ketone.
Examples of higher fatty acids include fatty acids having 12 to 30 carbon atoms such as lauric acid, myristic acid, pentadecyl acid, palmitic acid, palmitoleic acid, and stearic acid, with myristic acid, pentadecyl acid, palmitic acid, and stearic acid being preferred. .
Examples of the higher alcohol include alcohols having 12 to 30 carbon atoms, such as myristyl alcohol, cetyl alcohol (also known as cetanol), stearyl alcohol, and behenyl alcohol.
水不溶性粉末材料を適度な細孔容積を有する顆粒に顆粒化する観点から、水不溶性粉末材料に対する有機結合剤の質量比（有機結合剤／水不溶性粉末材料）は、好ましくは０．０２以上、より好ましくは０．１以上、更に好ましくは０．２５以上であり、粗大粒子を減少させて、歯垢除去性能を高める観点から、該質量比は、好ましくは５以下、より好ましくは２．５以下、更に好ましくは１．５以下である。該質量比は、好ましくは０．０２～５、より好ましくは０．１～２．５、更に好ましくは０．２５～１．５である。 From the viewpoint of granulating the water-insoluble powder material into granules having an appropriate pore volume, the mass ratio of the organic binder to the water-insoluble powder material (organic binder/water-insoluble powder material) is preferably 0.02 or more, More preferably, it is 0.1 or more, still more preferably 0.25 or more, and from the viewpoint of reducing coarse particles and improving plaque removal performance, the mass ratio is preferably 5 or less, more preferably 2.5. Below, it is more preferably 1.5 or less. The mass ratio is preferably 0.02 to 5, more preferably 0.1 to 2.5, and still more preferably 0.25 to 1.5.
（増粘剤）
本発明では、有機結合剤の粘度を増加させることにより、顆粒化における有機結合剤の吸収抑制を図り、歯磨剤用顆粒の細孔容積を高める観点から、増粘剤を用いることが好ましい。すなわち、増粘剤は、溶融状態の有機結合剤の粘度を高める機能を有する。
増粘剤は、天然高分子、半合成高分子、合成高分子等の分子量が１，０００を超える高分子が好ましい。分子量は、供給のし易さの観点から、１０万以下が好ましい。増粘剤は、多流体ノズルを用いて、容器回転型混合機中の水不溶性粉末材料に供給することが好ましく、有機結合剤と共に供給することがより好ましい。なお、増粘剤の分子量が分布を有する場合には、重量平均分子量が上記の範囲であることが好ましい。
増粘剤は、有機結合剤と共に、水不溶性粉末材料を適度な細孔容積を有する顆粒に顆粒化する観点から、その融点又は軟化点が好ましくは２５℃以上、より好ましくは３０℃以上、更に好ましくは４０℃以上、より更に好ましくは５０℃以上であり、ノズルからの吐出性や製造中の熱負荷の観点から、好ましくは１５０℃以下、より好ましくは１００℃以下、更に好ましくは９５℃以下、より更に好ましくは９０℃以下である。
増粘剤は、水不溶性粉末材料の結合剤としても機能することが好ましい観点から、疎水性であることが好ましい。疎水性であるとは、２５℃において、水１００ｇに対する溶解量が１ｇ以下であることを意味する。
増粘剤は、有機結合剤を添加する多流体ノズルとは、異なった多流体ノズルにより添加してもよく、同じ多流体ノズルから順次添加してもよく、増粘剤と有機結合剤とを予め混合して、多流体ノズルを用いて添加してもよい。適度な細孔容量を有する顆粒を製造する観点から、予め有機結合剤と増粘剤とを混合溶解してから多流体ノズルを用いて添加することが好ましく、予め有機結合剤と増粘剤とを均一に混合溶解してから多流体ノズルを用いて添加することがより好ましい。なお、有機結合剤と増粘剤との混合溶解の方法に限定はなく、任意の混合溶解条件を用いることができる。
(Thickener)
In the present invention, it is preferable to use a thickener from the viewpoint of increasing the viscosity of the organic binder to suppress absorption of the organic binder during granulation and increase the pore volume of the dentifrice granules. That is, the thickener has the function of increasing the viscosity of the molten organic binder.
The thickener is preferably a polymer having a molecular weight of over 1,000, such as a natural polymer, a semi-synthetic polymer, or a synthetic polymer. The molecular weight is preferably 100,000 or less from the viewpoint of ease of supply. The thickener is preferably fed to the water-insoluble powder material in the vessel rotary mixer using a multi-fluid nozzle, more preferably together with the organic binder. In addition, when the molecular weight of the thickener has a distribution, it is preferable that the weight average molecular weight is within the above range.
The thickener, together with the organic binder, preferably has a melting point or softening point of 25°C or higher, more preferably 30°C or higher, from the viewpoint of granulating the water-insoluble powder material into granules having an appropriate pore volume. Preferably, the temperature is 40°C or higher, even more preferably 50°C or higher, and from the viewpoint of jetting properties from the nozzle and heat load during manufacturing, it is preferably 150°C or lower, more preferably 100°C or lower, and even more preferably 95°C or lower. , and even more preferably 90°C or lower.
The thickener is preferably hydrophobic from the viewpoint that it also preferably functions as a binder for the water-insoluble powder material. Being hydrophobic means that the amount dissolved in 100 g of water is 1 g or less at 25°C.
The thickener may be added using a different multi-fluid nozzle from the multi-fluid nozzle that adds the organic binder, or may be added sequentially from the same multi-fluid nozzle. They may be mixed in advance and added using a multifluid nozzle. From the viewpoint of manufacturing granules having an appropriate pore volume, it is preferable to mix and dissolve the organic binder and the thickener beforehand and then add the organic binder and the thickener using a multifluid nozzle. It is more preferable to uniformly mix and dissolve and then add using a multifluid nozzle. Note that there is no limitation on the method of mixing and dissolving the organic binder and the thickener, and any mixing and dissolving conditions can be used.
具体的な増粘剤としては、（i）キサンタンガム、デキストリン、ゼラチン等の多糖類、及びそれらのエステル（例えば、デキストリン脂肪酸エステル、イヌリン脂肪酸エステル等の多糖脂肪酸エステル）やエーテル等の天然又は半合成高分子、天然ゴム、（ii）アクリル酸、アクリル酸エステル、メタクリル酸、メタクリル酸エステル、ヒドロキシメタクリル酸エステル、スチレン、酢酸ビニル、ビニルピロリドン、マレイン酸エステル、メチルビニルエーテル、α－オレフィン等の単独重合体、及びそれらの共重合体等の合成高分子、合成ゴム等が挙げられ、これらの中では、疎水性有機結合剤、例えば高級脂肪酸を使用する場合には、効果的に増粘する観点から、多糖脂肪酸エステルが好ましい。 Specific thickeners include (i) natural or semi-synthetic polysaccharides such as xanthan gum, dextrin, and gelatin, and their esters (e.g., polysaccharide fatty acid esters such as dextrin fatty acid ester and inulin fatty acid ester) and ethers; polymers, natural rubber, (ii) single polymers such as acrylic acid, acrylic esters, methacrylic acid, methacrylic esters, hydroxy methacrylic esters, styrene, vinyl acetate, vinyl pyrrolidone, maleic esters, methyl vinyl ether, α-olefins, etc. Examples include synthetic polymers such as polymers and copolymers thereof, synthetic rubbers, etc. Among these, when using hydrophobic organic binders such as higher fatty acids, from the viewpoint of effectively thickening , polysaccharide fatty acid esters are preferred.
また、（増粘剤／水不溶性粉末材料）の質量比は、有機結合剤と共に、水不溶性粉末材料を適度な細孔容積を有する顆粒に顆粒化する観点から、好ましくは０．００１以上、より好ましくは０．０１以上、更に好ましくは０．０５以上であり、粗大粒子を減少させて、歯垢除去性能を高める観点から、該質量比は、好ましくは１以下、より好ましくは０．５以下、更に好ましくは０．３以下である。
有機結合剤と増粘剤との質量比（有機結合剤／増粘剤）は、有機結合剤と共に、水不溶性粉末材料を適度な細孔容積を有する顆粒に顆粒化する観点から、好ましくは３０／１以下、より好ましくは２０／１以下、多流体ノズルからの吐出性の観点から、更に好ましくは１０／１以下であり、好ましくは１／１０以上、より好ましくは１／５以上、更に好ましくは１／１以上である。
In addition, the mass ratio of (thickener/water-insoluble powder material) is preferably 0.001 or more, and more Preferably it is 0.01 or more, more preferably 0.05 or more, and from the viewpoint of reducing coarse particles and improving plaque removal performance, the mass ratio is preferably 1 or less, more preferably 0.5 or less. , more preferably 0.3 or less.
The mass ratio of the organic binder and the thickener (organic binder/thickener) is preferably 30 from the viewpoint of granulating the water-insoluble powder material into granules having an appropriate pore volume together with the organic binder. /1 or less, more preferably 20/1 or less, from the viewpoint of ejection properties from a multifluid nozzle, still more preferably 10/1 or less, preferably 1/10 or more, more preferably 1/5 or more, even more preferably is 1/1 or more.
（その他の成分）
本発明においては、本発明の目的を損なわない範囲で、水不溶性粉末材料、有機結合剤、及び増粘剤以外の、その他の成分を含有していてもよい。具体的には、薬用成分、着色剤等が例示される。
薬用成分としては、虫歯予防剤、抗微生物剤、酵素、抗炎症剤、知覚過敏予防剤、歯垢形成抑制剤、殺菌剤、タバコヤニ除去剤等が挙げられる。
(Other ingredients)
In the present invention, other components than the water-insoluble powder material, organic binder, and thickener may be contained within a range that does not impair the object of the present invention. Specifically, medicinal ingredients, coloring agents, etc. are exemplified.
Examples of medicinal ingredients include caries preventive agents, antimicrobial agents, enzymes, anti-inflammatory agents, hypersensitivity preventive agents, plaque formation inhibitors, bactericidal agents, tobacco tar removers, and the like.
着色剤としては、酸化チタン、群青等が挙げられ、これらの着色剤を添加することにより審美的効果を付加することができる。
上記の他の配合成分は、単独で又は２種以上を組み合せて使用することができる。
Examples of the coloring agent include titanium oxide and ultramarine, and adding these coloring agents can add an aesthetic effect.
The other ingredients listed above can be used alone or in combination of two or more.
また、結合剤として、上述した有機結合剤に加えて、珪酸塩等の無機結合剤などを含有してもよい。
珪酸塩としては、珪酸ナトリウム及び珪酸カリウムが例示され、入手容易性の観点から、珪酸ナトリウムが好ましい。珪酸ナトリウムとしては、メタ珪酸ナトリウム（Ｎａ２ＳｉＯ３）、オルト珪酸ナトリウム（Ｎａ４ＳｉＯ４）、二珪酸ナトリウム（Ｎａ２Ｓｉ２Ｏ５）、四珪酸ナトリウム（Ｎａ２Ｓｉ４Ｏ９）及びそれらの水和物が挙げられる。
その他の水不溶性無機結合剤としては、水酸基を有する珪素系化合物、アルミニウム系化合物、カルシウム系化合物、マグネシウム系化合物等を用いることができる。その具体例としては、二酸化珪素の分散体であるコロイダルシリカ、メタ珪酸アルミン酸マグネシウム、合成珪酸アルミニウム、珪酸カルシウム、ベントナイト、モンモリロナイト、カオリン、水酸化アルミニウムゲル、アルミナゾル、合成ヒドロタルサイト、炭酸マグネシウム、酸化マグネシウム、水酸化マグネシウム等が挙げられる。
Moreover, in addition to the organic binder mentioned above, an inorganic binder such as a silicate may be contained as a binder.
Examples of silicates include sodium silicate and potassium silicate, with sodium silicate being preferred from the viewpoint of easy availability. Examples of sodium silicate include sodium metasilicate (Na 2 SiO 3 ), sodium orthosilicate (Na 4 SiO 4 ), sodium disilicate (Na 2 Si 2 O 5 ), sodium tetrasilicate (Na 2 Si 4 O 9 ), and the like. Examples include hydrates of
As other water-insoluble inorganic binders, silicon-based compounds having hydroxyl groups, aluminum-based compounds, calcium-based compounds, magnesium-based compounds, etc. can be used. Specific examples include colloidal silica, which is a dispersion of silicon dioxide, magnesium metasilicate aluminate, synthetic aluminum silicate, calcium silicate, bentonite, montmorillonite, kaolin, aluminum hydroxide gel, alumina sol, synthetic hydrotalcite, magnesium carbonate, Examples include magnesium oxide and magnesium hydroxide.
本発明の製造方法は、乾燥工程を行わなくてもよい観点から、珪酸ナトリウム、珪酸カリウム等の珪酸塩を実質上供給しないことが好ましく、本発明の歯磨剤用顆粒が、珪酸塩を実質上含まないことが好ましい。なお、「実質上含まない」とは、本発明の歯磨剤用顆粒（水分を除く）中の含有量が、１質量％以下、好ましくは０．１質量％以下、より好ましくは０質量％であることを意味する。 In the production method of the present invention, it is preferable that silicates such as sodium silicate and potassium silicate are not substantially supplied from the viewpoint that a drying step is not required. It is preferable not to include it. In addition, "substantially not containing" means that the content in the dentifrice granules (excluding water) of the present invention is 1% by mass or less, preferably 0.1% by mass or less, and more preferably 0% by mass. It means something.
歯磨剤用顆粒（水分を除く）中、その他の成分の合計含有量は、水不溶性粉末材料及び有機結合剤の固形分の合計量１００質量部に対して、好ましくは０～２０質量部、より好ましくは０～５質量部、更に好ましくは０～１質量部である。 In the dentifrice granules (excluding water), the total content of other components is preferably 0 to 20 parts by mass, based on 100 parts by mass of the total solid content of the water-insoluble powder material and organic binder. It is preferably 0 to 5 parts by weight, more preferably 0 to 1 part by weight.
（容器回転型混合機）
本発明においては、顆粒製造時に、顆粒に強いせん断を与えて圧密することのないようにするために、容器回転型混合機を用いる。
容器回転型混合機としては、ドラム型混合機及びパン型混合機が好ましい。ドラム型混合機としては、ドラム状の円筒が回転して処理を行うものであれば特に限定されない。水平又はわずかに傾斜させたドラム型混合機も使用可能である。これらの装置は、バッチ式、連続式のいずれの方式でもよい。
なお、水不溶性粉末材料を含む粉体と容器回転型混合機の内壁との間の壁面摩擦係数が小さく、粉体に十分な上昇運動力を加えることが困難な場合は、容器内壁に混合を補助するための複数個の邪魔板（バッフル）を設けることが好ましい。邪魔板を設けることにより、粉体に上昇運動を付与することが可能となり、粉体混合性及び固液混合性が向上する。
(container rotating mixer)
In the present invention, a container rotating type mixer is used in order to prevent the granules from being compacted by applying strong shear during granule production.
As the container rotation type mixer, a drum type mixer and a pan type mixer are preferable. The drum-type mixer is not particularly limited as long as it has a rotating drum-shaped cylinder to carry out processing. Horizontal or slightly inclined drum mixers can also be used. These devices may be either batch type or continuous type.
In addition, if the wall friction coefficient between the powder containing water-insoluble powder material and the inner wall of the container rotating mixer is small and it is difficult to apply sufficient upward movement force to the powder, mix it on the inner wall of the container. It is preferable to provide a plurality of baffles for assistance. By providing the baffle plate, it becomes possible to impart upward motion to the powder, improving powder mixability and solid-liquid mixability.
容器回転型混合機の運転条件としては、混合機内の水不溶性粉末材料をできるだけ均一に流動させ、撹拌できる条件であれば特に制限されない。良好な崩壊強度等を有する顆粒を得る観点から、下記式（１）で定義されるフルード数を０．００５以上とすることが好ましく、０．０１以上とすることがより好ましく、０．０５以上とすることが更に好ましく、非圧密の顆粒を得る観点から、その上限は、１．０以下とすることが好ましく、０．６以下とすることがより好ましく、０．４以下とすることが更に好ましい。
フルード数：Ｆｒ＝Ｖ／｛（Ｒ×ｇ）｝１／２ （１）
Ｖ：周速［ｍ／ｓ］
Ｒ：回転中心から回転物の円周までの半径［ｍ］
ｇ：重力加速度［ｍ／ｓ２］
なお、本体胴部の回転によって顆粒化が進行するドラム型混合機又はパン型混合機においては、Ｖ及びＲは本体胴部の値を用い、主翼や解砕翼を備えた横型又は竪型混合機においては、Ｖ及びＲは主軸の値を用い、解砕翼を備えたパン型混合機においては、Ｖ及びＲは解砕翼の値を用いることとする。
The operating conditions of the container-rotating mixer are not particularly limited as long as the water-insoluble powder material in the mixer can be fluidized and stirred as uniformly as possible. From the viewpoint of obtaining granules having good disintegration strength etc., the Froude number defined by the following formula (1) is preferably 0.005 or more, more preferably 0.01 or more, and 0.05 or more. More preferably, from the viewpoint of obtaining non-consolidated granules, the upper limit is preferably 1.0 or less, more preferably 0.6 or less, and even more preferably 0.4 or less. preferable.
Froude number: Fr=V/{(R×g)} 1/2 (1)
V: Circumferential speed [m/s]
R: Radius from the center of rotation to the circumference of the rotating object [m]
g: Gravitational acceleration [m/s 2 ]
In addition, in a drum-type mixer or a pan-type mixer in which granulation progresses by the rotation of the main body body, V and R use the values of the main body body, and in a horizontal or vertical mixer equipped with a main wing or crushing blade. For V and R, the values of the main shaft are used, and in the case of a pan-type mixer equipped with a crushing blade, V and R are the values of the crushing blade.
（多流体ノズル）
本発明においては、多流体ノズルを用いて有機結合剤を水不溶性粉末材料に供給する。多流体ノズルを用いることにより、その液滴を微細化して分散させることができる。
多流体ノズルとは、液体と微粒化用気体（エアー、窒素等）を独立の流路を通してノズル先端部近傍まで流通させて混合・微粒化するノズルであり、二流体ノズル、三流体ノズル、四流体ノズル（特開平０８－２８１１５５号公報、及び特開２００２－２４９５１２号公報参照）等を挙げることができる。また、有機結合剤と微粒化用気体の混合部は、ノズル先端部内で混合する内部混合型、又はノズル先端部外で混合する外部混合型のいずれであってもよい。
このような多流体ノズルとしては、スプレーイングシステムスジャパン株式会社製、株式会社共立合金製作所製、株式会社いけうち製等の内部混合型二流体ノズル、スプレーイングシステムスジャパン株式会社製、株式会社共立合金製作所製、株式会社アトマックス製等の外部混合型二流体ノズル、藤崎電機株式会社製の外部混合型四流体ノズル等が挙げられる。
(Multi-fluid nozzle)
In the present invention, a multifluid nozzle is used to feed the organic binder to the water-insoluble powder material. By using a multifluid nozzle, the droplets can be made fine and dispersed.
A multi-fluid nozzle is a nozzle that mixes and atomizes a liquid and atomizing gas (air, nitrogen, etc.) through independent channels to the vicinity of the nozzle tip. Examples include fluid nozzles (see JP-A-08-281155 and JP-A-2002-249512). Further, the mixing part for the organic binder and the atomization gas may be either an internal mixing type in which the organic binder and the atomization gas are mixed within the nozzle tip, or an external mixing type in which they are mixed outside the nozzle tip.
Examples of such multifluid nozzles include internal mixing two-fluid nozzles manufactured by Spraying Systems Japan Co., Ltd., Kyoritsu Gokin Seisakusho Co., Ltd., and Ikeuchi Co., Ltd.; Examples include external mixing type two-fluid nozzles manufactured by Alloy Seisakusho and Atmax Co., Ltd., external mixing type four-fluid nozzles manufactured by Fujisaki Electric Co., Ltd., and the like.
二流体ノズルを用いる場合、微粒化用気体の流量の調整は、微粒化用気体の噴霧圧の調整により行うのが容易である。微粒化用気体噴霧圧としては、液分散の観点から０．０１ＭＰａ以上が好ましく、設備負荷の観点から１．０ＭＰａ以下が好ましい。また、有機結合剤の噴霧圧としては特に制限はないが、設備負荷の観点から、例えば１．０ＭＰａ以下が好ましい。 When using a two-fluid nozzle, the flow rate of the atomization gas can be easily adjusted by adjusting the spray pressure of the atomization gas. The atomization gas spray pressure is preferably 0.01 MPa or more from the viewpoint of liquid dispersion, and preferably 1.0 MPa or less from the viewpoint of equipment load. Further, there is no particular restriction on the spray pressure of the organic binder, but from the viewpoint of equipment load, it is preferably 1.0 MPa or less, for example.
有機結合剤の液滴径の平均径は、好ましくは２１０μｍ以下、より好ましくは１５０μｍ以下、更に好ましくは１００μｍ以下であり、生産性の観点から、その下限は、好ましくは１μｍ以上、より好ましくは５μｍ以上、更に好ましくは１０μｍ以上、より更に好ましくは２０μｍ以上である。
多流体ノズルは１本以上であればよいが、２～２０本用いることもできる。
なお、当該有機結合剤の液滴径の平均径は体積基準で算出されるものであり、例えば、レーザー回折式粒度分布測定装置（Ｍａｌｖｅｒｎ Ｉｎｓｔｒｕｍｅｎｔｓ社製、スプレーテック）を用いて測定される値である。
The average droplet diameter of the organic binder is preferably 210 μm or less, more preferably 150 μm or less, even more preferably 100 μm or less, and from the viewpoint of productivity, the lower limit is preferably 1 μm or more, more preferably 5 μm. The thickness is more preferably 10 μm or more, and even more preferably 20 μm or more.
The number of multifluid nozzles may be one or more, but it is also possible to use 2 to 20 multifluid nozzles.
Note that the average droplet diameter of the organic binder is calculated on a volume basis, and is, for example, a value measured using a laser diffraction particle size distribution analyzer (Spraytec, manufactured by Malvern Instruments). be.
水不溶性粉末材料の温度は、適度な細孔容積を有する歯磨剤用顆粒を得る観点から、好ましくは０℃以上、より好ましくは５℃以上、更に好ましくは１０℃以上であり、生産性の観点から、好ましくは１００℃以下、より好ましくは６０℃以下、更に好ましくは５０℃以下である。
なお、有機結合剤の融点と、水不溶性粉末材料の温度との差（有機結合剤の融点－水不溶性粉末材料の温度）は、多流体ノズルにより噴霧された有機結合剤が水不溶性粉末材料上で速やかに固化し、水不溶性粉末材料への吸収が抑制され、水不溶性粉末材料の細孔が残存することで、所望の細孔容積を有する顆粒を得る観点から、好ましくは－３０℃以上、より好ましくは－１０℃以上、更に好ましくは５℃以上、より好ましくは１０℃以上であり、そして、多流体ノズルにより噴霧された有機結合剤が水不溶性粉末材料上で急速に固化せずに濡れ広がり、水不溶性粉末材料間の細孔が形成されることで、所望の細孔容積を有する顆粒を得る観点から、好ましくは９０℃以下、より好ましくは８０℃以下、更に好ましくは６５℃以下、より更に好ましくは５０℃以下である。
本発明の製造方法では、通常の転動造粒と異なり、水不溶性粉末材料が室温付近であっても、融点以上の有機結合剤を添加することで、適度な細孔容積を有する歯磨剤用顆粒を製造することができる。これは、多流体ノズルを用いて有機結合剤を微細に噴霧供給しているため、水不溶性粉末材料に濡れ広がるのが速く、有機結合剤の水不溶性粉末材料への吸収よりも固化がより速く進行し、細孔が生じるためと考えられる。更に、通常の転動造粒法等では、結合剤を撹拌翼のせん断力で分散させるため、結合剤が瞬時に固化すると分散が困難になるのに対し、噴霧凝集法では、結合剤を予め分散して供給するため、室温でも適度な細孔容積を有する歯磨剤用顆粒を製造することが可能である。
なお、水不溶性粉末材料の温度は、容器回転型混合機中、有機結合剤を供給し始めた際の水不溶性粉末材料の温度であり、有機結合剤を供給し始めた際の容器回転型混合機内の温度で近似できる。
The temperature of the water-insoluble powder material is preferably 0°C or higher, more preferably 5°C or higher, and still more preferably 10°C or higher, from the viewpoint of obtaining dentifrice granules having an appropriate pore volume, and from the viewpoint of productivity. , preferably 100°C or lower, more preferably 60°C or lower, and even more preferably 50°C or lower.
The difference between the melting point of the organic binder and the temperature of the water-insoluble powder material (melting point of the organic binder - temperature of the water-insoluble powder material) is the difference between the melting point of the organic binder and the temperature of the water-insoluble powder material. From the viewpoint of obtaining granules having a desired pore volume by solidifying rapidly at , suppressing absorption into the water-insoluble powder material and leaving pores in the water-insoluble powder material, the temperature is preferably -30°C or higher. The temperature is more preferably -10°C or higher, even more preferably 5°C or higher, and even more preferably 10°C or higher, and the organic binder sprayed by the multifluid nozzle wets the water-insoluble powder material without rapidly solidifying. From the viewpoint of obtaining granules having a desired pore volume by expanding and forming pores between the water-insoluble powder materials, preferably 90 ° C. or less, more preferably 80 ° C. or less, still more preferably 65 ° C. or less, Even more preferably, the temperature is 50°C or lower.
In the manufacturing method of the present invention, unlike normal rolling granulation, even when the water-insoluble powder material is near room temperature, by adding an organic binder with a melting point or higher, the dentifrice has an appropriate pore volume. Granules can be produced. Because the organic binder is finely sprayed using a multi-fluid nozzle, it spreads quickly on the water-insoluble powder material and solidifies more quickly than when the organic binder is absorbed into the water-insoluble powder material. This is thought to be due to the progress of the process and the formation of pores. Furthermore, in conventional rolling granulation methods, the binder is dispersed by the shear force of stirring blades, which makes dispersion difficult if the binder instantly solidifies, whereas in the spray agglomeration method, the binder is dispersed in advance. Since it is distributed and supplied, it is possible to produce dentifrice granules having an appropriate pore volume even at room temperature.
The temperature of the water-insoluble powder material is the temperature of the water-insoluble powder material when the organic binder starts to be fed in the container rotating mixer, and the temperature of the water-insoluble powder material when the organic binder starts to be fed into the container rotating mixer. It can be approximated by the temperature inside the aircraft.
有機結合剤を多流体ノズルを用いて供給する際の有機結合剤の温度は、噴霧の安定性の観点から、有機結合剤の融点以上であり、融点＋５℃以上が好ましく、融点＋１０℃以上がより好ましく、生産性の観点から、好ましくは融点＋７０℃以下、より好ましくは融点＋６０℃以下、更に好ましくは融点＋５０℃以下である。
下記式より求められる結合剤添加速度（質量％／分）は、適度な細孔容積を有する顆粒を形成する観点から、好ましくは２０質量％／分以下、より好ましくは１０質量％／分以下であり、その下限は、好ましくは０．１質量％／分以上、より好ましくは０．５質量％／分以上、更に好ましくは１質量％／分以上である。
結合剤添加速度（質量％／分）＝結合剤添加質量（ｇ）／（容器回転型混合機内に添加した水不溶性粉末材料質量（ｇ）×結合剤添加時間（分））×１００
The temperature of the organic binder when supplying the organic binder using a multi-fluid nozzle is higher than the melting point of the organic binder from the viewpoint of spray stability, preferably higher than the melting point +5°C, and preferably higher than the melting point +10°C. More preferably, from the viewpoint of productivity, the melting point is preferably +70°C or lower, more preferably the melting point +60°C or lower, and still more preferably the melting point +50°C or lower.
The binder addition rate (mass %/min) determined from the following formula is preferably 20 mass %/min or less, more preferably 10 mass %/min or less, from the viewpoint of forming granules with an appropriate pore volume. The lower limit thereof is preferably 0.1 mass %/min or more, more preferably 0.5 mass %/min or more, and even more preferably 1 mass %/min or more.
Binder addition rate (mass%/min) = Binder addition mass (g) / (Water-insoluble powder material mass (g) added into the container rotating mixer x Binder addition time (min)) x 100
（乾燥）
本発明においては、融点が２５℃以上の有機結合剤を用いているため、実質上、乾燥操作を行う必要はなく、歯磨剤用顆粒の安定性及び生産効率の観点から、乾燥操作を行わない方が好ましい。ここでの乾燥操作とは、６０℃以上の温度での乾燥工程である。
(dry)
In the present invention, since an organic binder with a melting point of 25°C or higher is used, there is virtually no need to perform a drying operation, and from the viewpoint of stability and production efficiency of dentifrice granules, no drying operation is performed. is preferable. The drying operation here is a drying process at a temperature of 60°C or higher.
得られる顆粒中の水分量は、湿式崩壊強度を高める観点から、好ましくは５質量％以下、より好ましくは３質量％以下、更に好ましくは２質量％以下であり、より更に好ましくは１質量％以下であり、生産性の観点から、好ましくは０．１質量％以上であり、より好ましくは０．２質量％以上である。顆粒中の水分量は、実施例記載の方法により求めることができる。湿式崩壊強度は、有機結合剤及び水不溶性粉末材料の種類に依存するが、同じ種類では、水分量が少ない方が、湿式崩壊強度は高くなる。 The moisture content in the resulting granules is preferably 5% by mass or less, more preferably 3% by mass or less, even more preferably 2% by mass or less, even more preferably 1% by mass or less, from the viewpoint of increasing wet disintegration strength. From the viewpoint of productivity, it is preferably 0.1% by mass or more, more preferably 0.2% by mass or more. The amount of water in the granules can be determined by the method described in the Examples. Wet collapse strength depends on the type of organic binder and water-insoluble powder material, but for the same type, the lower the moisture content, the higher the wet collapse strength.
［歯磨剤用顆粒］
本発明の歯磨剤用顆粒は、有機結合剤と水不溶性粉末材料とを含有する歯磨剤用顆粒であって、水不溶性粉末材料の含有量が３０～９５質量％であり、有機結合剤の含有量が５～７０質量％であり、直径０．１～１０μｍの細孔の容積が０．０７～１ｍＬ／ｇである。
本発明の歯磨剤用顆粒は、前記の製造方法で得られるものが好ましい。他の製造方法としては、例えば、前記有機結合剤と水不溶性粉末材料と油剤、必要に応じて水とを転動造粒や噴霧乾燥で顆粒化させた後に、油剤を溶媒に抽出し除去する等の方法で、細孔を有する顆粒を得てもよい。
なお、本発明の歯磨剤用顆粒に使用される有機結合剤、粉末材料の具体例及び好ましい範囲は、上述した本発明の歯磨剤用顆粒の製造方法で使用される有機結合剤及び粉末材料と同様である。
[Granules for toothpaste]
The dentifrice granules of the present invention are dentifrice granules containing an organic binder and a water-insoluble powder material, in which the content of the water-insoluble powder material is 30 to 95% by mass, and the content of the organic binder is 30 to 95% by mass. The amount is 5 to 70% by mass, and the volume of pores with a diameter of 0.1 to 10 μm is 0.07 to 1 mL/g.
The dentifrice granules of the present invention are preferably obtained by the above manufacturing method. Another manufacturing method includes, for example, granulating the organic binder, water-insoluble powder material, oil agent, and water if necessary by rolling granulation or spray drying, and then extracting and removing the oil agent with a solvent. Granules having pores may be obtained by the following methods.
The specific examples and preferred ranges of the organic binder and powder material used in the dentifrice granules of the present invention are the same as the organic binder and powder material used in the method for producing dentifrice granules of the present invention described above. The same is true.
本発明の歯磨剤用顆粒（水分を除く）及び本発明の製造方法により得られた歯磨剤用顆粒（水分を除く）中、水不溶性粉末材料の含有量は、研磨力を高める観点から、好ましくは３０質量％以上、より好ましくは４０質量％以上、更に好ましくは４５質量％以上であり、歯に対する損傷を抑制する観点から、その上限は、好ましくは９５質量％以下、より好ましくは９０質量％以下、更に好ましくは８０質量％以下である。歯磨剤用顆粒中、水不溶性粉末材料の含有量は、好ましくは３０～９５質量％、より好ましくは４０～９０質量％、更に好ましくは４５～８０質量％である。
本発明において、歯磨剤用顆粒中の各成分の含有量や質量比は、顆粒製造時の配合量から求めた計算値を用いることができる。
In the dentifrice granules of the present invention (excluding water) and the dentifrice granules (excluding water) obtained by the production method of the present invention, the content of the water-insoluble powder material is preferably from the viewpoint of increasing the polishing power. is 30% by mass or more, more preferably 40% by mass or more, even more preferably 45% by mass or more, and from the viewpoint of suppressing damage to teeth, the upper limit is preferably 95% by mass or less, more preferably 90% by mass. The content is preferably 80% by mass or less. The content of the water-insoluble powder material in the dentifrice granules is preferably 30 to 95% by mass, more preferably 40 to 90% by mass, and still more preferably 45 to 80% by mass.
In the present invention, for the content and mass ratio of each component in the dentifrice granules, calculated values determined from the blending amounts at the time of granule production can be used.
本発明の歯磨剤用顆粒（水分を除く）及び本発明の製造方法により得られた歯磨剤用顆粒（水分を除く）中、有機結合剤の含有量は、細孔を有する顆粒を得る観点から、好ましくは５質量％以上、より好ましくは１０質量％以上、更に好ましくは１５質量％以上であり、収率を高める観点から、その上限は、好ましくは８０質量％以下、より好ましくは７０質量％以下、更に好ましくは６０質量％以下である。歯磨剤用顆粒中、有機結合剤の含有量は、好ましくは５～８０質量％、より好ましくは１０～７０質量％、更に好ましくは１５～６０質量％である。
水不溶性粉末材料に対する有機結合剤の含有量の質量比の好ましい範囲は、前述のものと同じである。
The content of the organic binder in the dentifrice granules of the present invention (excluding water) and the dentifrice granules (excluding water) obtained by the production method of the present invention is determined from the viewpoint of obtaining granules with pores. , preferably 5% by mass or more, more preferably 10% by mass or more, even more preferably 15% by mass or more, and from the viewpoint of increasing the yield, the upper limit is preferably 80% by mass or less, more preferably 70% by mass. The content is preferably 60% by mass or less. The content of the organic binder in the dentifrice granules is preferably 5 to 80% by mass, more preferably 10 to 70% by mass, and even more preferably 15 to 60% by mass.
The preferred range of the mass ratio of the content of the organic binder to the water-insoluble powder material is the same as described above.
本発明の歯磨剤用顆粒及び本発明の製造方法により得られた歯磨剤用顆粒の細孔容積は、歯磨剤に配合して使用したとき、歯垢除去性能を高める観点から、直径０．１～１０μｍの細孔の容積が、好ましくは０．０７ｍＬ／ｇ以上、より好ましくは０．１ｍＬ／ｇ以上、更に好ましくは０．１１ｍＬ／ｇ以上であり、生産性、顆粒の強度の観点から、好ましくは１ｍＬ／ｇ以下、より好ましくは０．８ｍＬ／ｇ以下、更に好ましくは０．６ｍＬ／ｇ以下、より更に好ましくは０．５ｍＬ／ｇ以下である。直径０．１～１０μｍの細孔の容積は、容器回転型混合機内の水不溶性粉末材料へ供給する有機結合剤の液滴径を適宜調整したり、容器回転型混合機のフルード数を適宜調整することにより、上記の範囲内の数値を達成することができる。
なお、直径０．１～１０μｍの細孔の容積は、実施例に記載の方法により測定される。
本発明の歯磨剤用顆粒及び本発明の製造方法により得られた歯磨剤用顆粒は、適度な細孔容積を有することで、歯磨き時のブラッシングで顆粒が様々な粒子径の顆粒に崩壊することで、ハブラシの毛先が届かないような大きさの隙間にも顆粒が届き、歯垢除去性能が向上すると考えられる。
The pore volume of the dentifrice granules of the present invention and the dentifrice granules obtained by the production method of the present invention is 0.1 in diameter from the viewpoint of improving plaque removal performance when used in a dentifrice. The volume of ~10 μm pores is preferably 0.07 mL/g or more, more preferably 0.1 mL/g or more, even more preferably 0.11 mL/g or more, from the viewpoint of productivity and granule strength, Preferably it is 1 mL/g or less, more preferably 0.8 mL/g or less, still more preferably 0.6 mL/g or less, even more preferably 0.5 mL/g or less. The volume of the pores with a diameter of 0.1 to 10 μm can be determined by appropriately adjusting the droplet diameter of the organic binder supplied to the water-insoluble powder material in the container rotating mixer, or by appropriately adjusting the Froude number of the container rotating mixer. By doing so, a value within the above range can be achieved.
Note that the volume of pores with a diameter of 0.1 to 10 μm is measured by the method described in Examples.
The dentifrice granules of the present invention and the dentifrice granules obtained by the production method of the present invention have an appropriate pore volume, so that the granules can be disintegrated into granules of various particle sizes during tooth brushing. It is thought that the granules reach gaps that are too large for the bristles of a toothbrush to reach, improving plaque removal performance.
本発明の歯磨剤用顆粒及び本発明の製造方法により得られた歯磨剤用顆粒の平均粒子径は、十分な研磨力を有する観点から、好ましくは５０μｍ以上、より好ましくは７５μｍ以上、更に好ましくは１００μｍ以上であって、口腔中での異物感を抑制する観点から、好ましくは５００μｍ以下、より好ましくは３５０μｍ以下、更に好ましくは３００μｍ以下である。歯磨剤用顆粒の平均粒子径は、好ましくは５０～５００μｍ、より好ましくは７５～３５０μｍ、更に好ましくは１００～３００μｍである。
なお、平均粒子径は、実施例に記載の方法で測定することができる。
The average particle diameter of the dentifrice granules of the present invention and the dentifrice granules obtained by the production method of the present invention is preferably 50 μm or more, more preferably 75 μm or more, and even more preferably It is 100 μm or more, and from the viewpoint of suppressing the feeling of a foreign body in the oral cavity, it is preferably 500 μm or less, more preferably 350 μm or less, and still more preferably 300 μm or less. The average particle diameter of the dentifrice granules is preferably 50 to 500 μm, more preferably 75 to 350 μm, and still more preferably 100 to 300 μm.
Note that the average particle diameter can be measured by the method described in Examples.
［歯磨剤］
本発明の歯磨剤は、前記本発明の歯磨剤用顆粒又は本発明の歯磨剤用顆粒の製造方法により製造された歯磨剤用顆粒を含有するものである。歯磨剤用顆粒の含有量は、歯磨剤中に、好ましくは１質量％以上、より好ましくは３質量％以上、更に好ましくは５質量％以上であり、そして、好ましくは５０質量％以下、より好ましくは３０質量％以下、更に好ましくは１５質量％以下である。歯磨剤中の前記歯磨剤用顆粒の含有量が前記範囲内であると、口腔内で顆粒の触知ができて、みぞれ状の感触（シャリシャリ感）を与えるが、徐々に崩壊していき、清掃効果感を認知できるという特徴を有し、また、優れた歯垢除去効果を奏する。
[Toothpaste]
The dentifrice of the present invention contains the dentifrice granules of the present invention or the dentifrice granules produced by the method for producing dentifrice granules of the present invention. The content of the dentifrice granules is preferably 1% by mass or more, more preferably 3% by mass or more, even more preferably 5% by mass or more, and preferably 50% by mass or less, more preferably is 30% by mass or less, more preferably 15% by mass or less. When the content of the dentifrice granules in the dentifrice is within the above range, the granules are palpable in the oral cavity and give a sleet-like feel (crispy feeling), but gradually disintegrate, It has the characteristic that the cleaning effect can be perceived, and also has an excellent plaque removal effect.
歯磨剤の調製は常法により行うことができる。この際、歯磨剤に通常使用される他の成分、例えば、粘結剤、湿潤剤、甘味剤、界面活性剤、防腐剤、香料、薬用成分、着色剤、その他一般に使用されている、炭酸カルシウム等の歯磨剤用研磨剤、賦形剤等を配合することができる。
粘結剤としては、カルボキシメチルセルロースナトリウム、ポリアクリル酸ナトリウム、ヒドロキシエチルセルロース、増粘性シリカ、モンモリロナイト、カラギーナン、アルギン酸ナトリウム、グアガム、ペクチン等が挙げられる。
湿潤剤としては、ソルビット、プロピレングリコール、１，３ブチレングリコール、エチレングリコール、ポリエチレングリコール、ポリプロピレングリコール、キシキリット、マルチット、ラクチット、エリスリトール等が挙げられ、甘味剤としては、サッカリンナトリウム、ステビオサイド、タイマチン（ソーマチン）、アスパラチルフェニルアラニンメチルエステル等が挙げられる。
The dentifrice can be prepared by conventional methods. At this time, other ingredients commonly used in dentifrices, such as binders, humectants, sweeteners, surfactants, preservatives, fragrances, medicinal ingredients, coloring agents, and other commonly used calcium carbonate. Abrasives for dentifrice such as, excipients, etc. can be blended.
Examples of the binder include sodium carboxymethyl cellulose, sodium polyacrylate, hydroxyethyl cellulose, thickening silica, montmorillonite, carrageenan, sodium alginate, guar gum, and pectin.
Humectants include sorbitol, propylene glycol, 1,3-butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xyquilit, maltit, lactit, erythritol, etc. Sweeteners include saccharin sodium, stevioside, taimatin (thaumatin), etc. , asparatylphenylalanine methyl ester, and the like.
界面活性剤としては、ラウリル硫酸ナトリウム等のアルキル硫酸塩、アシルグルタミン酸ナトリウムやアシルサルコシン酸ナトリウム等のアシルアミノ酸の塩、ラウリルリン酸ナトリウム等のアルキルリン酸の塩類、蔗糖脂肪酸エステル、ソルビタン脂肪酸エステル、ポリオキシエチレン脂肪酸エステル等が挙げられる。
防腐剤としては、パラベン、ｐ－オキシ安息香酸メチル、ｐ－オキシ安息香酸エチル、ｐ－オキシ安息香酸プロピル、ｐ－オキシ安息香酸ブチル、安息香酸ナトリウム等が挙げられる。
香料としては、メントール及びメントールを含む天然物；バジル、カンファー、キャラウェイ、カルダモン、コリアンダー、ゼラニウム、ジンジャー、ローレル、ラベンダー、メース、ナツメグ、ペッパー、ローズ、ローズマリー、タイム、イランイラン、ジャスミン、バニラ、ヒソップ、ラバンジン、オリス、キャロットシード、ダバナ、エレミ、オスマンタスの精油及び抽出物；ボルネオール及びその誘導体；ヘリオトロピン；α－、β－、γ－、δ－イオノン及びこれらの誘導体；チモール、バニリン、エチルバニリン、マルトール並びにエチルマルトール等が挙げられる。
薬用成分及び着色剤としては、前記のものが挙げられる。
上記成分は、単独で又は２種以上を組み合わせて使用することができる。
Examples of surfactants include alkyl sulfates such as sodium lauryl sulfate, salts of acyl amino acids such as sodium acylglutamate and sodium acylsarcosinate, salts of alkyl phosphates such as sodium lauryl phosphate, sucrose fatty acid esters, sorbitan fatty acid esters, Examples include polyoxyethylene fatty acid ester.
Examples of preservatives include paraben, methyl p-oxybenzoate, ethyl p-oxybenzoate, propyl p-oxybenzoate, butyl p-oxybenzoate, sodium benzoate, and the like.
Flavoring agents include menthol and natural products containing menthol; basil, camphor, caraway, cardamom, coriander, geranium, ginger, laurel, lavender, mace, nutmeg, pepper, rose, rosemary, thyme, ylang-ylang, jasmine, vanilla. , hyssop, lavandin, orris, carrot seed, davana, elemi, osmanthus essential oils and extracts; borneol and its derivatives; heliotropin; α-, β-, γ-, δ-ionone and their derivatives; thymol, vanillin, Examples include ethyl vanillin, maltol, and ethyl maltol.
The medicinal ingredients and colorants include those mentioned above.
The above components can be used alone or in combination of two or more.
以下の実施例及び比較例において、「％」は特記しない限り「質量％」である。なお、各物性値の測定は、以下の方法により行った。
なお、表中の配合組成の数値は、固形分の値である。
In the following Examples and Comparative Examples, "%" means "% by mass" unless otherwise specified. In addition, the measurement of each physical property value was performed by the following method.
In addition, the numerical value of the composition in the table is the value of the solid content.
（１）水不溶性粉末材料の平均粒子径
レーザー回折／散乱式粒度分布測定装置（株式会社堀場製作所製、ＬＡ－９２０）にて、溶媒：イオン交換水、屈折率：１．２、循環速度４、循環３ｍｉｎの条件で測定した。
(1) Average particle diameter of water-insoluble powder material Using a laser diffraction/scattering particle size distribution analyzer (manufactured by Horiba, Ltd., LA-920), solvent: ion exchange water, refractive index: 1.2, circulation rate 4 The measurement was performed under the conditions of 3 minutes of circulation.
（２）有機結合剤の融点
融解した試料をガラス毛管（内径１．０ｍｍ、長さ５０ｍｍ、試料高さ１０ｍｍ）に入れ、１０℃以下で２４時間静置した。その後、１分間に１℃の速度で昇温を続け、試料が溶解し完全に透明になったときの温度を融点とした。
(2) Melting point of organic binder The molten sample was placed in a glass capillary tube (inner diameter 1.0 mm, length 50 mm, sample height 10 mm) and allowed to stand at 10° C. or lower for 24 hours. Thereafter, the temperature was continued to increase at a rate of 1° C. per minute, and the temperature at which the sample melted and became completely transparent was defined as the melting point.
（３）顆粒の水分量
試料２ｇをアルミ製の直径１０．５ｃｍの容器上に均一に散布し、その後、赤外線水分計（株式会社島津製作所製、ＭＯＣ６３ｕ）を用い、温度１０５℃、Ａｕｔｏの条件（測定値の変化量が、３０秒間で０．０５％以内になったときを最終測定値とみなして測定を終了）で揮発自由水分量を測定し、顆粒の水分量とした。
(3) Moisture content of granules 2 g of the sample was uniformly spread on an aluminum container with a diameter of 10.5 cm, and then an infrared moisture meter (manufactured by Shimadzu Corporation, MOC63u) was used at a temperature of 105°C under Auto conditions. (When the amount of change in the measured value became within 0.05% in 30 seconds, it was considered as the final measured value and the measurement was terminated.) The volatile free water content was measured and taken as the water content of the granules.
（４）顆粒の平均粒子径
ＪＩＳ Ｚ ８８０１－１（２０００年５月２０日制定、２００６年１１月２０日最終改正）規定の２０００、１４００、１０００、７１０、５００、３５５、２５０、１８０、１２５、９０、６３、４５μｍの篩を用いて５分間振動させた後、篩分け法による篩下質量分布について５０％平均径を算出し、これを平均粒子径とした。具体的には、ＪＩＳ Ｚ ８８０１－１（２０００年５月２０日制定、２００６年１１月２０日最終改正）規定の２０００、１４００、１０００、７１０、５００、３５５、２５０、１８０、１２５、９０、６３、４５μｍの篩を用いて受け皿上に目開きの小さな篩から順に積み重ね、最上部の２０００μｍの篩の上から５０ｇの顆粒を添加し、蓋をしてロータップ型ふるい振とう機（株式会社平工製作所製、タッピング１５６回／分、ローリング：２９０回／分）に取り付け、５分間振動させたあと、それぞれの篩及び受け皿上に残留した当該顆粒の質量を測定し、各篩上の当該顆粒の質量割合（％）を算出した。受け皿から順に目開きの小さな篩上の当該顆粒の質量割合を積算していき合計が５０％となる粒子径を平均粒子径とした。
(4) Average particle diameter of granules 2000, 1400, 1000, 710, 500, 355, 250, 180, 125 as specified in JIS Z 8801-1 (established on May 20, 2000, last revised on November 20, 2006) , 90, 63, and 45 μm sieves for 5 minutes, the 50% average diameter was calculated for the under-sieve mass distribution by the sieving method, and this was taken as the average particle diameter. Specifically, 2000, 1400, 1000, 710, 500, 355, 250, 180, 125, 90, 63. Using a 45 μm sieve, stack the sieves with the smallest opening on a saucer, add 50 g of granules from the top of the 2000 μm sieve, cover with a lid, and use a low-tap type sieve shaker (Heiwa Co., Ltd.). After vibrating for 5 minutes, the mass of the granules remaining on each sieve and saucer was measured, and the mass of the granules on each sieve was measured. The mass percentage (%) was calculated. The mass percentages of the granules on the sieves with small openings were integrated in order from the receiving tray, and the particle size at which the total was 50% was defined as the average particle size.
（５）顆粒の細孔容積
水銀圧入式ポロシメーター（micromeritics社製、AutoPore IV 9500）にて、サンプル質量：０．１６ｇ、低圧時:Evacuation Pressure ５０ｍｍＨｇ、Evacuation Time １ｍｉｎ、Mercury Filling Pressure ０．４９ｐｓｉａ（３．３８ｋＰａ）、Equilibration Time ５ｓｅｃ、高圧時Equilibration Time ５ｓｅｃ、の条件で測定を行った。
(5) Pore volume of granules Sample mass: 0.16 g, low pressure: Evacuation Pressure 50 mmHg, Evacuation Time 1 min, Mercury Filling Pressure 0.49 psia (3 .38 kPa), Equilibration Time 5 sec, and Equilibration Time 5 sec at high pressure.
（６）歯垢除去率
歯間モデル（φ４のパスツールピペットを５本並べ接着固定）の溝に赤い口紅（オーブ：ＲＤ３０５）を塗り込む。その後、余分な口紅を歯ブラシ（チェック、花王株式会社製）と食器洗い用洗剤を用いてブラッシング洗浄（赤色が出なくなるまで）した。実施例又は比較例で得られた顆粒を用い、表２に示す処方に従って各歯磨剤を調製した。各歯磨剤を歯間モデルの上に１ｇ取り、口紅が歯ブラシに付着しなくなるまで刷掃を行った。歯間モデルに残った口紅をエタノール９０ｍＬで１０分間超音波洗浄し、抽出液を５４０ｎｍにて吸光度を測定（Ａｂｓ）し、歯磨剤で刷掃後の吸光度測定値とした。
なお、歯磨剤を使用せずに、口紅が歯ブラシに付着しなくなるまで刷掃を行い、モデルに残った口紅をエタノール９０ｍＬで１０分間超音波洗浄し、抽出液を５４０ｎｍにて吸光度測定（Ａｂｓ）したものを標準の吸光度測定値とし、以下の計算式から歯垢除去率を算出した。
歯垢除去率（％）＝（標準の吸光度測定値－歯磨剤で刷掃後の吸光度測定値）／標準の吸光度測定値×１００（％）
(6) Plaque removal rate Apply red lipstick (Orb: RD305) to the grooves of the interdental model (5 φ4 Pasteur pipettes lined up and fixed with adhesive). Thereafter, excess lipstick was removed by brushing (until the red color disappeared) using a toothbrush (Check, manufactured by Kao Corporation) and dishwashing detergent. Each dentifrice was prepared using the granules obtained in the Examples or Comparative Examples according to the formulations shown in Table 2. One gram of each dentifrice was placed on the interdental model and brushed until the lipstick no longer adhered to the toothbrush. The lipstick remaining on the interdental model was ultrasonically cleaned with 90 mL of ethanol for 10 minutes, and the absorbance of the extract was measured at 540 nm (Abs), which was taken as the absorbance measurement value after brushing with toothpaste.
In addition, without using toothpaste, brush the lipstick until it no longer sticks to the toothbrush, wash the remaining lipstick on the model with 90 mL of ethanol for 10 minutes with ultrasonic cleaning, and measure the absorbance of the extract at 540 nm (Abs). The obtained value was used as the standard absorbance measurement value, and the plaque removal rate was calculated from the following formula.
Plaque removal rate (%) = (standard absorbance measurement value - absorbance measurement value after brushing with toothpaste) / standard absorbance measurement value x 100 (%)
［実施例１～５］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（ＰＱ社製、商品名：Ｓｏｒｂｏｓｉｌ ＡＣ３３、平均粒子径：５．６μｍ）３．５ｋｇを、邪魔板を有した７５Ｌドラム型混合機（φ４０ｃｍ×Ｌ６０ｃｍ）に投入し、ドラム回転数３０ｒ／ｍｉｎ、フルード数０．２、ドラム角度１２．６°の条件で混合しながら、予め加熱溶融させたパルミチン酸（花王株式会社製、商品名：ルナックＰ－９５、融点：６２．９℃）を外部混合型二流体ノズル１本（株式会社アトマックス製、ＢＮ－９０）を用いて、噴霧添加し顆粒化した。ノズルに供するエアは５０℃に加温した。パルミチン酸噴霧後、１分間混合を継続した後、ドラム型混合機から排出し、顆粒の物性評価を行った。結果を表１に示す。
[Examples 1 to 5]
3.5 kg of silica (manufactured by PQ, trade name: Sorbosil AC33, average particle size: 5.6 μm), which had been adjusted to a predetermined temperature in advance at the blending ratio and conditions shown in Table 1, was mixed in a 75 L drum type with a baffle plate. Palmitic acid (manufactured by Kao Corporation, product (name: Lunac P-95, melting point: 62.9°C) was added by spraying and granulated using one external mixing type two-fluid nozzle (BN-90, manufactured by Atmax Co., Ltd.). The air supplied to the nozzle was heated to 50°C. After spraying palmitic acid, mixing was continued for 1 minute, and then the granules were discharged from the drum mixer and the physical properties of the granules were evaluated. The results are shown in Table 1.
［実施例６］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（ＰＱ社製、商品名：Ｓｏｒｂｏｓｉｌ ＡＣ３３、平均粒子径：５．６μｍ）３．５ｋｇを、邪魔板を有した７５Ｌドラム型混合機（φ４０ｃｍ×Ｌ６０ｃｍ）に投入し、ドラム回転数３０ｒ／ｍｉｎ、フルード数０．２、ドラム角度１２．６°の条件で混合しながら、予め加熱して溶融させたパルミチン酸（花王株式会社製、商品名：ルナックＰ－９５）とパルミチン酸デキストリン（千葉製粉株式会社製、商品名：レオパールＫＬ２、融点：５０～１３０℃）との混合液を、外部混合型二流体ノズル１本（株式会社アトマックス製、ＢＮ－９０）を用いて、噴霧添加し顆粒化した。ノズルに供するエアは５０℃に加温した。混合液噴霧後、１分間混合を継続した後、ドラム型混合機から排出し、顆粒の物性評価を行った。結果を表１に示す。
[Example 6]
3.5 kg of silica (manufactured by PQ, trade name: Sorbosil AC33, average particle size: 5.6 μm), which had been adjusted to a predetermined temperature in advance at the blending ratio and conditions shown in Table 1, was mixed in a 75 L drum type with a baffle plate. Palmitic acid (manufactured by Kao Corporation) was heated and melted while mixing under the conditions of a drum rotation speed of 30 r/min, a Froude number of 0.2, and a drum angle of 12.6°. , product name: Lunac P-95) and palmitic acid dextrin (manufactured by Chiba Flour Milling Co., Ltd., product name: Leopard KL2, melting point: 50 to 130°C) using one external mixing type two-fluid nozzle (Co., Ltd. The mixture was added by spraying and granulated using Atomax BN-90). The air supplied to the nozzle was heated to 50°C. After spraying the mixed solution, mixing was continued for 1 minute, and then the granules were discharged from the drum mixer and the physical properties of the granules were evaluated. The results are shown in Table 1.
［実施例７］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（Ｅｖｏｎｉｋ社製、商品名：Ｚｅｏｄｅｎｔ１２４、平均粒子径：９．８μｍ）３ｋｇを用い、パルミチン酸に替えて予め加熱溶融させたラウリン酸（花王株式会社製、商品名：ルナックＬ－９８、融点：４３．２℃）を用いたこと以外は、実施例１～５と同様に顆粒を製造し、顆粒の物性評価を行った。結果を表１に示す。
[Example 7]
Using 3 kg of silica (manufactured by Evonik, trade name: Zeodent 124, average particle size: 9.8 μm), which had been adjusted to a predetermined temperature in advance at the blending ratio and conditions shown in Table 1, laurin, which had been heated and melted in place of palmitic acid, was used. Granules were produced in the same manner as in Examples 1 to 5, except that acid (manufactured by Kao Corporation, trade name: Lunac L-98, melting point: 43.2°C) was used, and the physical properties of the granules were evaluated. The results are shown in Table 1.
［実施例８］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（Ｅｖｏｎｉｋ社製、商品名：Ｚｅｏｄｅｎｔ１２４、平均粒子径：９．８μｍ）３ｋｇを用い、パルミチン酸に替えて予め加熱溶融させたステアリン酸（花王株式会社製、商品名：ルナックＳ－９８、６９．９℃）を用いたこと以外は、実施例１～５と同様に顆粒を製造し、顆粒の物性評価を行った。結果を表１に示す。
[Example 8]
Using 3 kg of silica (manufactured by Evonik, product name: Zeodent 124, average particle size: 9.8 μm), which was adjusted to a predetermined temperature in advance at the blending ratio and conditions shown in Table 1, stearin was heated and melted in place of palmitic acid. Granules were produced in the same manner as in Examples 1 to 5, except that acid (manufactured by Kao Corporation, trade name: Lunac S-98, 69.9°C) was used, and the physical properties of the granules were evaluated. The results are shown in Table 1.
［実施例９］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（Ｅｖｏｎｉｋ社製、商品名：Ｚｅｏｄｅｎｔ１２４、平均粒子径：９．８μｍ）３ｋｇを用い、パルミチン酸に替えて予め加熱溶融させたセタノール（花王株式会社製、商品名：カルコール６０９８、融点：４９．３℃）を用いたこと以外は、実施例１～５と同様に顆粒を製造し、顆粒の物性評価を行った。結果を表１に示す。
[Example 9]
Using 3 kg of silica (manufactured by Evonik, trade name: Zeodent 124, average particle size: 9.8 μm), which had been adjusted to a predetermined temperature in advance at the blending ratio and conditions shown in Table 1, cetanol, which had been heated and melted in place of palmitic acid, was used. (manufactured by Kao Corporation, trade name: Calcol 6098, melting point: 49.3°C), except that granules were produced in the same manner as in Examples 1 to 5, and the physical properties of the granules were evaluated. The results are shown in Table 1.
［実施例１０］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（Ｅｖｏｎｉｋ社製、商品名：Ｚｅｏｄｅｎｔ１２４、平均粒子径：９．８μｍ）３ｋｇを用い、パルミチン酸に替えて予め加熱溶融させたキャンデリラワックス（横関油脂工業株式会社製、商品名：精製キャンデリラワックスＭＫ－２、融点：６８～７２℃）を用いたこと以外は、実施例１～５と同様に顆粒を製造し、顆粒の物性評価を行った。結果を表１に示す。
[Example 10]
Using 3 kg of silica (manufactured by Evonik, trade name: Zeodent 124, average particle size: 9.8 μm), which had been adjusted to a predetermined temperature in advance at the blending ratio and conditions shown in Table 1, a can was heated and melted in place of palmitic acid. Granules were produced in the same manner as in Examples 1 to 5, except that Delilah wax (manufactured by Yokozeki Oil Industry Co., Ltd., trade name: purified Candelilla wax MK-2, melting point: 68 to 72°C) was used. Physical properties were evaluated. The results are shown in Table 1.
［比較例１］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（比較例１：ＰＱ社製、商品名：Ｓｏｒｂｏｓｉｌ ＡＣ３３、平均粒子径：５．６μｍ）３．５ｋｇを、邪魔板を有した７５Ｌドラム型混合機（φ４０ｃｍ×Ｌ６０ｃｍ）に投入し、ドラム回転数３０ｒ／ｍｉｎ、フルード数０．２、ドラム角度１２．６°の条件で混合しながら、珪酸ナトリウム水溶液（富士化学工業株式会社製、商品名：３号珪酸ソーダ：Ｎａ２Ｏ・３ＳｉＯ２水溶液、固形分：５５．１％）を外部混合型二流体ノズル１本（株式会社アトマックス製、ＢＮ－９０）を用いて、噴霧添加し顆粒化した。ノズルに供するエアは室温条件とした。珪酸ナトリウム水溶液噴霧後、１分間混合を継続した後、ドラム型混合機から排出し、電気式棚乾燥機（アドバンテック株式会社製、ＤＲＭ６２０ＴＢ）を用いて１２０℃で４時間乾燥した後、顆粒の物性評価を行った。結果を表１に示す。
[Comparative example 1]
Using the blending ratio and conditions shown in Table 1, 3.5 kg of silica (Comparative Example 1: manufactured by PQ, trade name: Sorbosil AC33, average particle diameter: 5.6 μm), which had been adjusted to a predetermined temperature in advance, was mixed with a baffle plate. A sodium silicate aqueous solution (manufactured by Fuji Chemical Industry Co., Ltd.) was added to a 75L drum-type mixer (φ40cm x L60cm) and mixed under the conditions of a drum rotation speed of 30 r/min, a Froude number of 0.2, and a drum angle of 12.6°. , product name: No. 3 sodium silicate : Na 2 O. It was added and granulated. The air supplied to the nozzle was kept at room temperature. After spraying the sodium silicate aqueous solution, mixing was continued for 1 minute, the drum mixer was discharged, and after drying at 120°C for 4 hours using an electric shelf dryer (manufactured by Advantech Co., Ltd., DRM620TB), the physical properties of the granules were determined. We conducted an evaluation. The results are shown in Table 1.
［比較例２］
表１に示す配合割合及び条件で、予め所定温度に調整したシリカ（ＰＱ社製、商品名：Ｓｏｒｂｏｓｉｌ ＡＣ３３、平均粒子径：５．６μｍ）３００ｇを２Ｌハイスピードミキサー（深江パウテック株式会社製）に投入し、アジテータ回転数８５０ｒ／ｍｉｎ、チョッパー回転数１，５００ｒ／ｍｉｎ、ジャケット温水温度８０℃の条件で２分間混合した後、予め加熱溶融させたパルミチン酸（花王株式会社製、商品名：ルナックＰ－９５、融点：６２．９℃）を添加し顆粒化した。パルミチン酸添加後、１分間混合を継続した後、ハイスピードミキサーから排出し、顆粒の物性評価を行った。結果を表１に示す。
[Comparative example 2]
Using the blending ratio and conditions shown in Table 1, 300 g of silica (manufactured by PQ, trade name: Sorbosil AC33, average particle size: 5.6 μm), which had been adjusted to a predetermined temperature, was placed in a 2L high-speed mixer (manufactured by Fukae Powtech Co., Ltd.). After mixing for 2 minutes at an agitator rotation speed of 850 r/min, a chopper rotation speed of 1,500 r/min, and a jacket hot water temperature of 80°C, heat-melted palmitic acid (manufactured by Kao Corporation, product name: Lunac) was added. P-95 (melting point: 62.9°C) was added and granulated. After addition of palmitic acid, mixing was continued for 1 minute, and then the mixture was discharged from the high-speed mixer, and the physical properties of the granules were evaluated. The results are shown in Table 1.
［歯垢除去率の評価］
上述した評価方法に従い、表２に示す処方に従って歯磨剤組成物を調製し、表２に示す歯磨剤組成物９２質量部に対して実施例２の歯磨剤用顆粒８質量部を混合した歯磨剤を用いて評価を行なった。
その結果、実施例２の歯磨剤用顆粒を含有する歯磨剤は、十分な歯垢除去率を示すことが確認された。
[Evaluation of plaque removal rate]
According to the evaluation method described above, a dentifrice composition was prepared according to the formulation shown in Table 2, and 8 parts by mass of the dentifrice granules of Example 2 were mixed with 92 parts by mass of the dentifrice composition shown in Table 2. The evaluation was conducted using
As a result, it was confirmed that the dentifrice containing the dentifrice granules of Example 2 exhibited a sufficient plaque removal rate.
表２において使用した成分は以下の通りである。
＊１ 無水珪酸：サイロピュア２５、富士シリシア化学株式会社製
The components used in Table 2 are as follows.
*1 Silicic anhydride: Silopure 25, manufactured by Fuji Silysia Chemical Co., Ltd.
本発明の歯磨剤用顆粒の製造方法は、製造効率に優れ、更に、該製造方法により得られた顆粒は、適度な細孔容積を有する。本発明により得られた歯磨剤用顆粒は、歯磨剤に配合した際、効果的に歯垢を除去することができる。 The method for producing dentifrice granules of the present invention has excellent production efficiency, and furthermore, the granules obtained by the method have an appropriate pore volume. The dentifrice granules obtained according to the present invention can effectively remove dental plaque when incorporated into a dentifrice.
Claims (8)
該有機結合剤の融点が２５℃以上１５０℃以下であり、
該工程において、多流体ノズルを用いて、水不溶性粉末材料に有機結合剤を供給する、歯磨剤用顆粒の製造方法であって、
該有機結合剤が、油脂、ワックス、高級脂肪酸、及び高級アルコールから選ばれる１種以上であり、
該水不溶性粉末材料に対する該有機結合剤の質量比（有機結合剤／水不溶性粉末材料）が、０．０２以上５以下であり、
該歯磨剤用顆粒が珪酸塩を実質上含まない、歯磨剤用顆粒の製造方法。 A step of mixing a water-insoluble powder material and an organic binder heated to a temperature above the melting point using a container rotating mixer,
The melting point of the organic binder is 25°C or more and 150°C or less ,
A method for producing dentifrice granules, wherein the step uses a multifluid nozzle to supply an organic binder to a water-insoluble powder material, the method comprising:
The organic binder is one or more selected from oils and fats, waxes, higher fatty acids, and higher alcohols,
The mass ratio of the organic binder to the water-insoluble powder material (organic binder/water-insoluble powder material) is 0.02 or more and 5 or less,
A method for producing dentifrice granules, wherein the dentifrice granules are substantially free of silicate.
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