JP3166273B2 - Method for refining microcrystalline cellulose product - Google Patents
Method for refining microcrystalline cellulose productInfo
- Publication number
- JP3166273B2 JP3166273B2 JP5869992A JP5869992A JP3166273B2 JP 3166273 B2 JP3166273 B2 JP 3166273B2 JP 5869992 A JP5869992 A JP 5869992A JP 5869992 A JP5869992 A JP 5869992A JP 3166273 B2 JP3166273 B2 JP 3166273B2
- Authority
- JP
- Japan
- Prior art keywords
- crystalline cellulose
- cellulose product
- product
- microcrystalline cellulose
- manufactured
- 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.)
- Expired - Fee Related
Links
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、結晶セルロース製品の
微細化方法に関する。利用分野としては、食品，化粧
品，工業分野等に幅広く利用することができる。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for refining crystalline cellulose products. It can be widely used in food, cosmetics, industrial fields, and the like.
【０００２】[0002]
【従来の技術】一般に粉体を微細化する方法としては、
卓上ニーダー，回転ボールミル，振動ボールミル，コロ
イドミル，バンタムミル，ビーズミル，ホモジナイザー
等が挙げられる。例えば、特公昭６２―３０２２０号公
報には、ホモジナイザーを用いて微結晶セルロース懸濁
液を高圧均質化処理することで、安定な分散性と高い粘
性を示す懸濁液が得られると記載されている。ここで言
う均質化処理とは、少なくとも２００ｋｇ／ｃｍ2 、好
ましくは３５０〜５６０ｋｇ／ｃｍ2 の圧力差で小径オ
リフィスを通過させて加速し、次にこれを衝突させて急
速に減速させることにより、剪断および切断を行わせる
工程を繰り返すことである。加速時の速度は最大２００
ｍ／秒とされている。2. Description of the Related Art In general, methods for making powder finer include:
A table kneader, a rotary ball mill, a vibrating ball mill, a colloid mill, a bantam mill, a bead mill, a homogenizer and the like can be used. For example, Japanese Patent Publication No. Sho 62-30220 describes that a suspension exhibiting stable dispersibility and high viscosity can be obtained by subjecting a microcrystalline cellulose suspension to high-pressure homogenization treatment using a homogenizer. I have. Homogenization here means accelerating through a small diameter orifice with a pressure difference of at least 200 kg / cm @ 2, preferably 350-560 kg / cm @ 2, and then impinging on it to rapidly decelerate and shear. This is to repeat the process of cutting. Speed up to 200 when accelerating
m / sec.
【０００３】しかしながら、従来の技術では結晶セルロ
ース製品を微細化しようとしてもある粒径以下には進行
しない、また微細化するのに低いスラリー濃度しかでき
ない，時間がかかる（何回もパスする必要がある）等の
問題があった。[0003] However, in the prior art, the micronization of the crystalline cellulose product does not proceed below a certain particle size, and a low slurry concentration is required for the micronization, and it takes time (multiple passes are required). A)).
【０００４】[0004]
【発明が解決しようとする課題】本発明者等は、上記課
題を解決すべく鋭意検討した結果本発明に到達したもの
である。即ち本発明の目的は、結晶セルロース製品を効
率良く、平均粒径数μｍ程度まで微細化する方法を提供
することである。The present inventors have made intensive studies to solve the above-mentioned problems, and have reached the present invention. That is, an object of the present invention is to provide a method for efficiently refining a crystalline cellulose product to an average particle size of about several μm.
【０００５】[0005]
【課題を解決するための手段】本発明は、スラリー濃度
１〜２０ｗｔ％の結晶セルロース製品水系分散液を、微
細オリフィス内で片側流速２００ｍ／秒以上の流速で対
面衝突させることを特徴とする結晶セルロース製品の微
細化方法に関するものである。本発明の実施に用いられ
る装置としては、超高圧破砕装置、例えば「ナノマイザ
ー」〈登録商標〉システム（ナノマイザー（株）製）が
適している。ナノマイザーシステムでは、貫通孔２孔と
それらを連結する溝を持つ２枚のディスクに加圧供給さ
れた結晶セルロース製品が、微細オリフィス内で加速さ
れ、高速で対面衝突することにより微細化される。従っ
て、衝突速度が低いと効率良く微細化されず、本発明の
実施に際しては結晶セルロース製品を２００ｍ／秒以上
に加速する必要がある。この場合、結晶セルロース製品
スラリーは、５００ｋｇ／ｃｍ2以上に加圧して供給さ
れる。According to the present invention, there is provided a crystallization method wherein a crystalline cellulose product aqueous dispersion having a slurry concentration of 1 to 20 wt% is face-to-face collision in a fine orifice at a flow rate of 200 m / sec or more on one side. The present invention relates to a method for miniaturizing a cellulose product. As an apparatus used for carrying out the present invention, an ultra-high pressure crushing apparatus, for example, “Nanomizer” (registered trademark) system (manufactured by Nanomizer Co., Ltd.) is suitable. In the nanomizer system, a crystalline cellulose product pressurized and supplied to two disks having two through-holes and a groove connecting them is accelerated in a fine orifice, and is refined by face-to-face collision at a high speed. . Therefore, when the collision speed is low, the micronization is not efficiently performed, and in practicing the present invention, it is necessary to accelerate the crystalline cellulose product to 200 m / sec or more. In this case, the crystalline cellulose product slurry is supplied under a pressure of 500 kg / cm 2 or more.
【０００６】本発明で言う結晶セルロース製品とは、結
晶セルロース及びその複合体のことである。結晶セルロ
ースはインダストリアル・アンド・エンジニアリング・
ケミストリー、第４２巻、第５０２〜５０７頁（１９５
０）に記載されているオー・エー・バチスタ氏の報文に
よって定義されているものであって、セルロースを酸加
水分解又はアルカリ酸化分解して得られる実質的に一定
の重合度を有するセルロース結晶子集合物である。例え
ば、セルロースを２．５規定の塩酸で１０５℃，１５分
間加水分解処理すると一定重合度を有する酸不溶解残渣
を生成し、これを洗浄，濾過すると結晶セルロースが得
られる。また、結晶セルロース複合体は、特公昭５７―
１４７７１号に記載されている複合体を指し、結晶セル
ロースと水溶性のガム類等の分散剤及びデンプン分解物
等の崩壊剤を、水分の存在下で磨砕練合し、乾燥したも
のである。[0006] The crystalline cellulose product referred to in the present invention refers to crystalline cellulose and its complex. Microcrystalline cellulose is manufactured by Industrial & Engineering
Chemistry, Vol. 42, pp. 502-507 (195
A cellulose crystal having a substantially constant degree of polymerization obtained by acid hydrolysis or alkali oxidative degradation of cellulose, which is defined by the report of O.A. It is a child aggregate. For example, when cellulose is hydrolyzed with 2.5 N hydrochloric acid at 105 ° C. for 15 minutes, an acid-insoluble residue having a certain degree of polymerization is generated, and the residue is washed and filtered to obtain crystalline cellulose. In addition, the crystalline cellulose composite is available from
No. 14771, which is obtained by grinding and kneading crystalline cellulose, a dispersing agent such as a water-soluble gum, and a disintegrating agent such as a starch decomposed product in the presence of moisture and drying. .
【０００７】結晶セルロースに該当するものとして、市
販品では「アビセル」〈登録商標〉ＦＤ−１０１，ＴＧ
−１０１（旭化成工業（株）製）等が挙げられ、また、
結晶セルロース複合体に該当するものとして、市販品で
は「アビセル」〈登録商標〉ＲＣ−Ｎ８１，ＲＣ−Ｎ３
０，ＲＣ−５９１（旭化成工業（株）製）等が挙げられ
る。[0007] As a product equivalent to crystalline cellulose, a commercially available product is "Avicel" (registered trademark) FD-101, TG
-101 (manufactured by Asahi Kasei Corporation) and the like.
As a product corresponding to the crystalline cellulose composite, “Avicel” (registered trademark) RC-N81, RC-N3 is a commercially available product.
0, RC-591 (manufactured by Asahi Kasei Corporation).
【０００８】本発明において、結晶セルロース製品スラ
リーの濃度は１〜２０ｗｔ％である。なぜなら、スラリ
ー濃度が１ｗｔ％未満では実用的でなく、２０ｗｔ％を
超えると微細化効率が低下するからである。また、結晶
セルロースの場合は予備的に微細化して、体積平均粒径
（粒子全体の体積に対して積算体積が５０％になる時の
粒子の球形換算直径）を１５μｍ以下にしておくことが
望ましい。[0008] In the present invention, the concentration of the crystalline cellulose product slurry is 1 to 20 wt%. This is because if the slurry concentration is less than 1 wt%, it is not practical, and if it exceeds 20 wt%, the miniaturization efficiency is reduced. Further, in the case of crystalline cellulose, it is desirable that the volume average particle diameter (the spherical equivalent diameter of the particles when the integrated volume becomes 50% with respect to the total volume of the particles) be 15 μm or less in advance. .
【０００９】尚、体積平均粒径の測定は、ＨＯＲＩＢＡ
レーザー回折式粒度分布測定装置（ＬＡ―５００型，
（株）堀場製作所製）を用いた。Incidentally, the measurement of the volume average particle diameter is carried out by HORIBA
Laser diffraction particle size distribution analyzer (LA-500 type,
(Manufactured by Horiba Ltd.).
【００１０】[0010]
【実施例】以下、実施例により本発明を具体的に説明す
る。The present invention will be described below in detail with reference to examples.
【００１１】[0011]
【実施例１〜２】結晶セルロース複合体「アビセル」
〈登録商標〉ＲＣ−Ｎ８１（旭化成工業（株）製）の１
５ｗｔ％水分散スラリーを調製し、微細オリフィス内の
片側流速を変えて超高圧破砕装置「ナノマイザー」〈登
録商標〉システム（ＬＡ―１１型，ナノマイザー（株）
製）で処理した。ＲＣ−Ｎ８１スラリーの処理前の体積
平均粒径は１５．０μｍであった。結果を表１に示す。
結晶セルロースは体積平均粒径数μｍ程度まで効率良く
微細化された。Examples 1-2: Crystalline cellulose composite "Avicel"
<Registered trademark> RC-N81 (manufactured by Asahi Kasei Corporation)
A 5 wt% aqueous dispersion slurry was prepared, and the ultra-high pressure crusher "Nanomizer"<registeredtrademark> system (LA-11 type, Nanomizer Co., Ltd.) was prepared by changing the flow rate on one side in the fine orifice.
Manufactured). The volume average particle size of the RC-N81 slurry before treatment was 15.0 μm. Table 1 shows the results.
The crystalline cellulose was efficiently refined to a volume average particle size of about several μm.
【００１２】[0012]
【比較例１〜３】結晶セルロース複合体「アビセル」
〈登録商標〉ＲＣ−Ｎ８１（旭化成工業（株）製）の２
５ｗｔ％水分散スラリーを調製し、実施例１〜２と同様
の方法で処理した。ＲＣ−Ｎ８１スラリーの処理前の体
積平均粒径は１５．２μｍであった。結果を表１に示
す。スラリー濃度１５ｗｔ％の場合と比較して、微細化
効率が低下した。Comparative Examples 1 to 3 Crystalline Cellulose Complex "Avicel"
<Registered trademark> RC-N81 (manufactured by Asahi Chemical Industry Co., Ltd.)
A 5 wt% aqueous dispersion slurry was prepared and treated in the same manner as in Examples 1 and 2. The volume average particle size of the RC-N81 slurry before treatment was 15.2 μm. Table 1 shows the results. The miniaturization efficiency was reduced as compared with the case where the slurry concentration was 15 wt%.
【００１３】[0013]
【実施例３〜４】結晶セルロース「アビセル」〈登録商
標〉ＦＤ−１０１（旭化成工業（株）製）の１５ｗｔ％
水分散スラリーを調製し、実施例１〜２と同様の方法で
処理した。ＦＤ−１０１スラリーの処理前の体積平均粒
径は２５．１μｍであった。結果を表２に示す。結晶セ
ルロースは体積平均粒径数μｍ程度まで効率良く微細化
された。Examples 3 and 4 15 wt% of crystalline cellulose "Avicel" (registered trademark) FD-101 (manufactured by Asahi Kasei Corporation)
An aqueous dispersion slurry was prepared and treated in the same manner as in Examples 1-2. The volume average particle size of the FD-101 slurry before treatment was 25.1 μm. Table 2 shows the results. The crystalline cellulose was efficiently refined to a volume average particle size of about several μm.
【００１４】[0014]
【実施例５】結晶セルロース「アビセル」〈登録商標〉
ＦＤ−１０１（旭化成工業（株）製）を、バンタムミル
で予備破砕し体積平均粒径１４．５μｍにした。その後
１５ｗｔ％水分散スラリーを調製し、実施例１〜２と同
様の方法で処理した。結果を表２に示す。予備破砕する
ことで、微細化効率が向上した。Example 5 Microcrystalline cellulose "Avicel" (registered trademark)
FD-101 (manufactured by Asahi Kasei Corporation) was pre-crushed with a bantam mill to have a volume average particle size of 14.5 μm. Thereafter, a 15 wt% aqueous dispersion slurry was prepared and treated in the same manner as in Examples 1 and 2. Table 2 shows the results. Pre-crushing improved the micronization efficiency.
【００１５】[0015]
【比較例４〜６】結晶セルロース複合体「アビセル」
〈登録商標〉ＲＣ−Ｎ８１（旭化成工業（株）製）の１
５ｗｔ％水分散スラリーを調製し、マントン・ガウリン
ホモジナイザーを用いて５００ｋｇ／ｃｍ2 の圧力差で
５回パスさせた。ＲＣ−Ｎ８１スラリーの処理前の体積
平均粒径は１５．０μｍであった。結果を表３に示す。
結晶セルロースを数μｍ程度まで微細化することはでき
なかった。Comparative Examples 4-6 Crystalline cellulose composite "Avicel"
<Registered trademark> RC-N81 (manufactured by Asahi Kasei Corporation)
A 5 wt% aqueous dispersion slurry was prepared and passed five times using a Manton-Gaulin homogenizer with a pressure difference of 500 kg / cm2. The volume average particle size of the RC-N81 slurry before treatment was 15.0 μm. Table 3 shows the results.
Crystalline cellulose could not be miniaturized to about several μm.
【００１６】[0016]
【表１】 [Table 1]
【００１７】[0017]
【表２】 [Table 2]
【００１８】[0018]
【表３】 [Table 3]
【００１９】[0019]
【発明の効果】本発明の微細化方法を用いることで、結
晶セルロース製品を効率良く、平均粒径数μｍ程度まで
微細化することができる。According to the method of the present invention, the crystalline cellulose product can be efficiently refined to an average particle size of about several μm.
Claims (1)
ロース製品水系分散液を、微細オリフィス内で片側流速
２００ｍ／秒以上の流速で対面衝突させることを特徴と
する結晶セルロース製品の微細化方法。1. A method for refining a crystalline cellulose product, comprising subjecting an aqueous dispersion of a crystalline cellulose product having a slurry concentration of 1 to 20 wt% to face-to-face collision in a fine orifice at a flow rate of 200 m / sec or more on one side.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5869992A JP3166273B2 (en) | 1992-03-17 | 1992-03-17 | Method for refining microcrystalline cellulose product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5869992A JP3166273B2 (en) | 1992-03-17 | 1992-03-17 | Method for refining microcrystalline cellulose product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05255513A JPH05255513A (en) | 1993-10-05 |
| JP3166273B2 true JP3166273B2 (en) | 2001-05-14 |
Family
ID=13091779
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5869992A Expired - Fee Related JP3166273B2 (en) | 1992-03-17 | 1992-03-17 | Method for refining microcrystalline cellulose product |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3166273B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20160026490A (en) | 2014-09-01 | 2016-03-09 | 전영채 | Strap for dish racks |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20000055131A (en) * | 1999-02-03 | 2000-09-05 | 유현식 | Method for preparing metaloxide slurry for semiconductor element cmp |
| JP6999291B2 (en) * | 2017-05-25 | 2022-01-18 | 昭和産業株式会社 | Mix for takoyaki or okonomiyaki, and manufacturing method for takoyaki or okonomiyaki |
-
1992
- 1992-03-17 JP JP5869992A patent/JP3166273B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20160026490A (en) | 2014-09-01 | 2016-03-09 | 전영채 | Strap for dish racks |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05255513A (en) | 1993-10-05 |
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