JPH0665417A - Fine particulate cellulosic raw material composition containing water - Google Patents

Fine particulate cellulosic raw material composition containing water

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Publication number
JPH0665417A
JPH0665417A JP4221088A JP22108892A JPH0665417A JP H0665417 A JPH0665417 A JP H0665417A JP 4221088 A JP4221088 A JP 4221088A JP 22108892 A JP22108892 A JP 22108892A JP H0665417 A JPH0665417 A JP H0665417A
Authority
JP
Japan
Prior art keywords
water
weight
raw material
fine particulate
present
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.)
Granted
Application number
JP4221088A
Other languages
Japanese (ja)
Other versions
JP3423334B2 (en
Inventor
Yuichi Komuro
雄一 小室
Ryotaro Kusakabe
亮太郎 草壁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Asahi Chemical Industry Co Ltd
Original Assignee
Asahi Chemical Industry Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Asahi Chemical Industry Co Ltd filed Critical Asahi Chemical Industry Co Ltd
Priority to JP22108892A priority Critical patent/JP3423334B2/en
Publication of JPH0665417A publication Critical patent/JPH0665417A/en
Application granted granted Critical
Publication of JP3423334B2 publication Critical patent/JP3423334B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PURPOSE:To provide the fine particulate cellulosic raw material composition containing water comprising a specific fine particulate cellulosic raw material, water and a dispersion auxiliary, improved in its transportation efficiency, capable of being readily dispersed by a usual stirring operation, and useful in the fields of foods, etc. CONSTITUTION:This sludge-like fine particulate celluosic raw material composition containing water having a water content of 0.17-3% is produced by removing water from a mixture by an evaporation method, spraying method, hot air method, etc., the mixture being obtained by mixing (A) 1 pt.wt. of a fine particulate cellulosic raw material, (B)>=3 pts.wt. of water, and (C) >=0.01 pt.wt., preferably <=1 pt.wt., of a dispersion auxiliary (e.g. a dextrin compound, glucose), the diameters of the particles occupying 50 integrated volume % of the component A being 0.3-6mum, and the integrated volume ratio of the particles having diameters of <=3mum being <=25%. The composition is efficiently transported in comparison with conventional suspensions, is good in dispersibility when redispersed in water, and is readily stirred and dispersed without requiring a homogenizer, etc.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、食品分野、化粧品分
野、コーティング分野、製膜分野、塗料分野、製紙分野
等全産業分野で巾広く利用価値を有する微粒子化された
セルロース系素材の供給形態に関する発明である。
[Field of Industrial Application] The present invention is in the form of supply of finely divided cellulosic material which has wide utility value in all industrial fields such as food field, cosmetic field, coating field, film-forming field, coating field and paper-making field. It is an invention related to.

【0002】[0002]

【従来の技術】セルロースを微細な粒子にする事は難し
く、常法、例えばボールミルやハンマーミル、コロイド
ミル、三本ロールミル、ホモジナイザー等で粉砕しても
平均粒径は10μm近辺までしか微細化されなかった。
最近,本発明者等により特開平3−163135号公報
の方法により、積算体積50%の粒径が0.3〜6μm
であり、かつ3μm以下の粒子の積算体積割合が25%
以上となる迄微粒子化されたセルロース系素材を懸濁液
の状態で得られるようになった。この微粒化セルロース
系素材の懸濁液、特にその水性懸濁液は、独特な滑らか
な感触と流動特性により、多方面の産業分野での展開が
指向されておりその有用性は明らかである。
2. Description of the Related Art It is difficult to make cellulose into fine particles, and even if it is pulverized by a conventional method such as a ball mill, a hammer mill, a colloid mill, a three-roll mill, a homogenizer, etc., the average particle diameter is reduced to about 10 μm. There wasn't.
Recently, according to the method disclosed in Japanese Patent Laid-Open No. 3-163135 by the present inventors, the particle size with an integrated volume of 50% is 0.3 to 6 μm.
And the cumulative volume ratio of particles of 3 μm or less is 25%
Until the above, the finely divided cellulosic material can be obtained in the state of suspension. The suspension of the micronized cellulosic material, especially the aqueous suspension thereof, is directed to development in various industrial fields due to its unique smooth feel and flow characteristics, and its usefulness is clear.

【0003】しかるに、この懸濁液を輸送するにあたっ
ては、多くの水分を含有している為、輸送効率が低く、
この改善が要望されていた。又、水分量が多いと腐敗に
対する抵抗が劣り用途によっては品質上問題があった。
本発明者は微粒化セルロース系素材の水懸濁液を乾燥
し、粉体化した後に水へ再分散させてみたが、元の微粒
子にまで戻すにはホモジナイザー等の強烈なシェアによ
る攪拌磨砕が必要であり、これは使用者にとっては面倒
な事となる。また、乾燥するにあたり、高分子ガム類や
デンプン分解物などの物質をあらかじめ混入させると、
乾燥後の粉体の水への再分散は若干改善されるものの、
沈降性粒子が存在して、元の状態に完全には戻らず、や
はりホモジナイザー等の強烈な攪拌が必須となる。
However, when this suspension is transported, since it contains a large amount of water, the transportation efficiency is low,
This improvement was requested. Further, when the water content is large, the resistance to rotting is poor and there is a quality problem depending on the application.
The present inventor has dried an aqueous suspension of micronized cellulosic material, pulverized it and then re-dispersed it in water, but in order to return it to the original fine particles, it is stirred and ground by a strong shear such as a homogenizer. Is necessary, which is troublesome for the user. Also, when drying, if substances such as polymer gums and starch decomposition products are mixed in advance,
Although the redispersion of powder in water after drying is slightly improved,
Since the settling particles are present, the state is not completely returned to the original state, and intense stirring with a homogenizer or the like is also essential.

【0004】[0004]

【発明が解決しようとする課題】本発明の目的は、水中
に戻して、通常の攪拌で容易に分散し、本来の微粒化セ
ルロース懸濁液の具備する性能を再現出来る組成物を提
供する事である。本発明の別の目的は、微粒化されたセ
ルロース系素材を輸送するにあたり、輸送の効率が改善
された組成物を提供する事である。
SUMMARY OF THE INVENTION An object of the present invention is to provide a composition which can be easily dispersed by returning it to water and ordinary stirring to reproduce the performance of the original micronized cellulose suspension. Is. Another object of the present invention is to provide a composition having an improved transportation efficiency in transporting the atomized cellulosic material.

【0005】[0005]

【課題を解決するための手段】本発明者等は、上記の課
題を解決する為に鋭意検討を重ねた結果、輸送の効率が
改善され、かつ通常の攪拌で容易に分散する、微粒化セ
ルロース系素材の組成物を見出し、本発明を完成するに
至り、これにより供給形態と使い勝手が改良されて産業
上の利用価値が増々高まる事となる。
Means for Solving the Problems The inventors of the present invention have conducted extensive studies to solve the above-mentioned problems, and as a result, the efficiency of transportation is improved, and the finely divided cellulose is easily dispersed by ordinary stirring. The present invention has been completed by finding out the composition of the system material, and by this, the supply form and the usability are improved, and the industrial utility value is increased more and more.

【0006】すなわち本発明は、積算体積50%の粒径
が0.3〜6μmであり、かつ3μm以下の粒子の積算
体積割合が25%以上である微粒化セルロース系素材1
重量部に対し、水を0.17〜3重量部、分散補助剤を
0.01重量部以上含有することを特徴とする微粒化セ
ルロース系素材含水組成物である。本発明でのセルロー
ス系素材とは、セルロースを含有する素材を表すもので
あり、例えば、木材、パルプ、リンターパルプ、竹パル
プ、バガスパルプのような脱リグニン処理を施した精製
パルプであったり、またはコットン繊維、コットンリン
ター、麻繊維のようなセルロース系天然繊維であった
り、またはそれらに脱リグニン処理を施した精製天然繊
維であったり、またはビスコースや銅アンモニア溶液か
ら凝固再生された再生セルロース成形物であったり、ま
たは穀物又は果実由来の食物繊維(例えば、小麦フス
マ、えん麦フスマ、とうもろこし外皮、米ぬか、ビール
粕、大豆粕、えんどう豆繊維、おから、リンゴ繊維な
ど)であったり、または木材や稲ワラに代表されるよう
なリグノセルロース材料であったりする。これらセルロ
ース系素材が、セルロースI型の結晶形をしたセルロー
スもしくは食物繊維である場合には、天然物と見做され
て何らの安全上の心配や法的規制も無く食用に供され
る。これらセルロース系素材がセルロースII型の結晶
形をしたセルロースである場合には、微粒化された粒子
の膨潤性が増し、保水性が更に向上する。これらセルロ
ース系素材がリグノセルロース材料である場合において
も同様であり、例えば木材チップ等は本発明によって始
めて微小な粒子となり、その懸濁液は濃厚感の有るペー
スト状物となるのである。
That is, according to the present invention, a micronized cellulosic material 1 having a particle size of 0.3 to 6 μm in an integrated volume of 50% and an integrated volume ratio of particles of 3 μm or less of 25% or more.
A microparticulate cellulose-based material hydrous composition comprising 0.17 to 3 parts by weight of water and 0.01 part by weight or more of a dispersion aid with respect to parts by weight. The cellulosic material in the present invention represents a material containing cellulose, for example, wood, pulp, linter pulp, bamboo pulp, refined pulp subjected to delignification treatment such as bagasse pulp, or Cellulose natural fibers such as cotton fibers, cotton linters, and hemp fibers, or purified natural fibers obtained by subjecting them to delignification treatment, or regenerated cellulose molding coagulated and regenerated from viscose or copper ammonia solution. Foods derived from cereals or fruits (for example, wheat bran, oat bran, corn hulls, rice bran, beer meal, soybean meal, pea fiber, okara, apple fiber, etc.), or It may be a lignocellulosic material such as wood or rice straw. When these cellulosic materials are cellulosic type I crystalline form cellulose or dietary fiber, they are regarded as natural products and are used for food without any safety concerns or legal restrictions. When these cellulosic materials are cellulosic II type crystalline cellulose, the swelling property of the atomized particles is increased and the water retention is further improved. The same applies when these cellulosic materials are lignocellulosic materials. For example, wood chips and the like become fine particles for the first time in accordance with the present invention, and the suspension thereof becomes a paste-like material having a thick feeling.

【0007】本発明での積算体積50%の粒径とは、粒
子全体の体積に対して積算体積が50%になるときの粒
子の球形換算直径のことで、メジアン径とも呼ばれる。
本発明の微粒化セルロース系素材の積算体積50%の粒
径は、0.3〜6μmである。6μmを越えると微粒化
セルロースとしての特異な性質を有さず、ざらつきがあ
り、沈降が見られる。又、積算体積50%の粒径は、小
さいほど良いが製造上0.3μm以上である。
The particle size with an integrated volume of 50% in the present invention is the spherical equivalent diameter of a particle when the integrated volume is 50% with respect to the volume of the entire particle, and is also called the median diameter.
The particle size of the micronized cellulosic material of the present invention in an integrated volume of 50% is 0.3 to 6 μm. When it exceeds 6 μm, it does not have the peculiar properties as micronized cellulose, it is rough, and sedimentation is observed. Further, the smaller the particle size with an integrated volume of 50%, the better, but it is 0.3 μm or more in terms of manufacturing.

【0008】又、3μm以下の粒子の積算体積割合と
は、3μm以下の粒子の合計体積の、全粒子の合計体積
に対する割合を百分率で示した値の事である。本発明で
は、再分散したときに粘調な懸濁液を得るために、3μ
m以下の粒子の積算体積割合が25%以上である必要が
ある。本発明組成物は、微粒化セルロース系素材1重量
部に対し水が0.17〜3重量部である。(以下、〜部
と表現する場合はすべて微粒化セルロース系素材を1重
量部としての比率を表わす事とする。)従来の懸濁液
(特開平3−163135号公報)では、懸濁液濃度2
重量%以上であるので、微粒化セルロース系素材に対し
水が50重量部にもなるような組成物であり、従来の懸
濁液に較べて本発明の組成物は輸送の効率が改善され
る。又、微粒化セルロース系素材1重量部に対して、水
が0.17重量部を下廻る迄水分を飛ばしてしまった本
発明外の組成物は分散補助剤の存在にもかかわらず水へ
の完全な再分散には前述のごとくホモジナイザーを必要
とする。
Further, the cumulative volume ratio of particles of 3 μm or less is a value showing the ratio of the total volume of particles of 3 μm or less to the total volume of all particles in percentage. In the present invention, in order to obtain a viscous suspension when redispersed,
The cumulative volume ratio of particles of m or less needs to be 25% or more. The composition of the present invention contains water in an amount of 0.17 to 3 parts by weight per 1 part by weight of the atomized cellulosic material. (Hereinafter, the term "-part" means the ratio of 1 part by weight of the finely divided cellulosic material.) In the conventional suspension (JP-A-3-163135), the suspension concentration is Two
Since the content is more than 50% by weight, the composition is such that water is as much as 50 parts by weight with respect to the micronized cellulosic material, and the composition of the present invention has improved transport efficiency as compared with conventional suspensions. . Further, the composition outside the present invention, which has lost water until the amount of water falls below 0.17 parts by weight with respect to 1 part by weight of the finely divided cellulosic material, is A homogenizer as described above is required for complete redispersion.

【0009】本発明の組成物のように、水が0.17〜
3重量部の物を得るには、1例としては特開平3−16
3135号公報の懸濁液中に後述する分散補助剤を0.
01重量部以上含有せしめた後に、水分を何らかの方法
により除去してゆけば良い。最も一般的には蒸発法で、
いわゆる乾燥工程を経て行けば良く、噴霧法、ベルト
法、ドラム法、高周波法、真空法、熱風法等いずれの方
式でも可能であるが、大切なのは水が0.17重量部を
下廻る迄水分を飛ばしてしまわない事である。更には、
水が0.17重量部を下廻る迄水分を飛ばしてしまった
後に水分を付加して0.17〜3重量部の範囲に再び持
っていっても再分散性は改善されず、水分の除去に際し
てはその履歴上で0.17重量部を切らさない事が、本
発明の組成物を得る為の重要な特徴である。
Like the composition of the present invention, the water content is 0.17-.
To obtain 3 parts by weight, as an example, JP-A-3-16
In the suspension of Japanese Patent No. 3135, a dispersion auxiliary agent to be described later was added.
It is sufficient to remove the water by some method after the content of 01 parts by weight or more. Most commonly by evaporation,
What is necessary is to go through a so-called drying process, and any method such as a spray method, a belt method, a drum method, a high frequency method, a vacuum method, a hot air method, etc. can be used, but it is important that the water content is less than 0.17 parts by weight. The thing is that you don't skip. Furthermore,
Even if water is added until the water falls below 0.17 parts by weight and water is added to bring it to the range of 0.17 to 3 parts by weight, the redispersibility is not improved and the removal of water In that case, it is an important feature for obtaining the composition of the present invention that 0.17 parts by weight in history is not cut off.

【0010】水分を除去してゆく他の方法は、遠心力を
利用するもの、逆浸透膜や半透膜を利用するもの、水の
凍結現象を利用するものなどが有る。又、本発明の組成
物は分散補助剤を0.01部以上含有する。この分散補
助剤は、水分を0.17〜3重量部にまで除去する前に
微粒化セルロース系素材とよくなじませておく。つま
り、水を3重量部以上、分散補助剤を0.01重量部以
上含む混合物を用意し、その混合物から前述の水分除去
手段等を用いる事によって、本発明の組成物である水分
が0.17〜3重量部の含水組成物とするのである。分
散補助剤無しでは、水への再分散が容易な物は出来な
い。分散補助剤は0.01重量部以上と言う少量で効果
を発揮するが、これは水分が0.17重量部を下廻る迄
水分除去を行わないからである。
Other methods of removing water include a method utilizing centrifugal force, a method utilizing a reverse osmosis membrane or a semipermeable membrane, and a method utilizing a freezing phenomenon of water. Further, the composition of the present invention contains 0.01 part or more of a dispersion aid. This dispersion aid is mixed well with the atomized cellulosic material before removing water to 0.17 to 3 parts by weight. That is, by preparing a mixture containing 3 parts by weight or more of water and 0.01 parts by weight or more of a dispersion aid, and using the above-mentioned water removing means or the like from the mixture, the water content of the composition of the present invention is 0. It is 17 to 3 parts by weight of the water-containing composition. Without a dispersion aid, a product that can be easily redispersed in water cannot be obtained. The dispersion auxiliary agent is effective in a small amount of 0.01 parts by weight or more, because the water is not removed until the water content falls below 0.17 parts by weight.

【0011】本発明の含水組成物の水への再分散性と言
う観点からは、分散補助剤の含有量は多くてもかまわな
いが、あまりに多量であると微粒化セルロース系素材の
供給形態と言う本発明組成物の本来の目的を逸脱してし
まう事となるので、分散補助剤は1重量部迄とするのが
通常である。本発明の分散補助剤とは、グルコース、ブ
ドウ糖、庶糖、果糖、乳糖、麦芽糖、セロビオース、セ
ロトリオース、セロテトラオース、マルトトリオース、
フラクトース、キシロース、各種オリゴ糖、ソルビッ
ト、デキストリン類、デンプン類、ソルボース、ガム分
解物、各種ガム類、プルラン、カードラン、寒天、ペク
チン、デキストラン、ゼラチン、セルロース誘導体、ア
ルギン酸、ファーセレラン、マルメロ、等の水溶性物質
又は水膨潤性物質である。
From the viewpoint of the redispersibility of the water-containing composition of the present invention in water, the content of the dispersion aid may be large, but if the content is too large, the finely divided cellulosic material is supplied in a form. Since it deviates from the original purpose of the composition of the present invention, it is usual that the amount of the dispersion aid is 1 part by weight. The dispersion aid of the present invention, glucose, glucose, sucrose, fructose, lactose, maltose, cellobiose, cellotriose, cellotetraose, maltotriose,
Fructose, xylose, various oligosaccharides, sorbit, dextrins, starches, sorbose, gum decomposition products, various gums, pullulan, curdlan, agar, pectin, dextran, gelatin, cellulose derivatives, alginic acid, furceleran, quince, etc. It is a water-soluble substance or a water-swellable substance.

【0012】これらは、水分を除去して行った時に、セ
ルロース系微粒子同志の表面水酸基の水素結合による凝
集を防止すると考えるが、水分子のようにセルロース系
微粒子の内部にまでは浸入せず粒子表面を薄くコーティ
ングする。次に、実施例により本発明を詳細に説明する
が、本発明は、これらに限定されるものではない。
These are considered to prevent the aggregation of the surface hydroxyl groups of the cellulosic fine particles due to the hydrogen bond when the water is removed, but the particles do not penetrate into the inside of the cellulosic fine particles like water molecules. Thinly coat the surface. Next, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto.

【0013】また、実施例中、微粒化セルロース系素材
の積算体積50%の粒径、3μm以下の粒子の積算体積
割合を決定する際粒径の測定は以下の方法で行った。島
津製作所製レーザー回折式粒度分布測定装置(SALD
−1100型)を用いて、測定に供する懸濁液を蒸留水
でセルロース系素材の濃度が0.1重量%となるように
希釈し、装置に内蔵する超音波発信器で粒子の2次凝集
を壊した状態で測定する。測定にあたっては、測定レン
ジを0.1〜45μmに設定し、これにより、ミー(M
ie)散乱理論式(測定装置中に組み込まれている)か
ら導き出された散乱強度と粒子径の関係を用いて計算さ
れる。また屈折率は1.7〜0.2iの標準屈折率用を
選択することとし、粒度分布を求める計算方法は最小二
乗法理論を使った直接計算法を使うこととする。1つの
試料に対する測定回数は7回に指定し、測定間隔は2秒
とする。セルロース系素材が0.1重量%に蒸留水で均
一に希釈された試料は、フローセルを利用して測定され
るが、内蔵された超音波発信器は常時オンとし、少なく
とも1分以上は超音波をあてて、凝集が進行するのを防
止した後に測定を行う。水への再分散性は、本発明組成
物へ蒸留水を加えてセルロース系素材濃度を5.0重量
%とし、これを強烈攪拌の例としてはエースホモジナイ
ザー(日本精機製AM−T)にて15000rpmで2
分間攪拌分散させ、軽度攪拌の例としてはスクリュー型
攪拌翼にて3000rpmで10分間攪拌分散させた。
その後、前述の手法で粒度測定を行って、元の粒度と比
較する事により水への再分散性を評価した。
In the examples, the particle size was measured by the following method when determining the particle size of the micronized cellulosic material at an integrated volume of 50% and the integrated volume ratio of particles of 3 μm or less. Shimadzu laser diffraction particle size distribution analyzer (SALD
-1100 type) is used to dilute the suspension to be used for measurement with distilled water so that the concentration of the cellulosic material is 0.1% by weight, and the secondary agglomeration of the particles is carried out with an ultrasonic transmitter incorporated in the device. Measure with the broken. In the measurement, the measurement range was set to 0.1 to 45 μm, which allowed me (M
ii) Calculated using the relationship between the scattering intensity and the particle size derived from the theoretical scattering formula (built into the measuring device). The refractive index is selected to be 1.7 to 0.2i for the standard refractive index, and the calculation method for obtaining the particle size distribution is to use the direct calculation method using the least square method theory. The number of measurements for one sample is specified as 7 and the measurement interval is 2 seconds. A sample in which the cellulosic material is uniformly diluted to 0.1% by weight with distilled water is measured by using a flow cell. The built-in ultrasonic transmitter is always on, and the ultrasonic wave is kept for at least 1 minute or more. Is applied to prevent aggregation from proceeding, and then the measurement is performed. For redispersibility in water, distilled water was added to the composition of the present invention to make the concentration of the cellulosic material 5.0% by weight. As an example of vigorous stirring, an ace homogenizer (AM-T manufactured by Nippon Seiki Co., Ltd.) was used. 2 at 15000 rpm
The mixture was stirred and dispersed for 1 minute, and as an example of mild stirring, the mixture was stirred and dispersed at 3000 rpm for 10 minutes with a screw type stirring blade.
Then, the particle size was measured by the above-mentioned method, and the redispersibility in water was evaluated by comparing with the original particle size.

【0014】[0014]

【実施例】本発明を下記実施例により説明するが、これ
らは本発明の範囲を制限するものではない。
The present invention is illustrated by the following examples, which do not limit the scope of the present invention.

【0015】[0015]

【実施例1〜4】針葉樹サルファイト法溶解パルプ(N
−DSP)を52℃で濃度18%の苛性ソーダ溶液に浸
漬後圧搾してセルロース濃度33重量%のアルカリセル
ロースとした。これを酸素濃度50%の雰囲気で48℃
で168時間アルカリ酸化分解し、次いで水洗洗浄を行
ってアルカリ分を除去した後、加水してスラリー状に
し、アシザワ株式会社製パールミル(商品名)で湿式粉
砕して微粒化セルロース系素材の水性懸濁液を得た。こ
の水性懸濁液に分散補助剤として市販デキストリン(松
谷化学株式会社製、商品名パインデックス)の種々の濃
度の水溶液を添加混合し、微粒化セルロース系素材濃度
5.0重量%、デキストリン0.05重量%、0.5重
量%、2.0重量%、5.0重量%、水が夫々94.9
5重量%、94.5重量%、93重量%、90重量%の
組成の混合物を得た。これらの混合物中のセルロース系
素材の積算体積50%粒径は1.7μm、3μm以下の
粒子の積算体積割合は72.1%であった。次にこれら
の混合物を目皿に取り、マントルヒーター上で攪拌しな
がら加熱して水分を蒸発させ、水分が0.7〜0.8重
量部となるまで水分除去を続けた。このようにして得ら
れたスラッジ様の本発明組成物1〜4の水への再分散性
を測定した。
Examples 1 to 4 Softwood sulfite method dissolving pulp (N
-DSP) was dipped in a caustic soda solution having a concentration of 18% at 52 ° C and then pressed to obtain alkali cellulose having a cellulose concentration of 33% by weight. This is 48 ° C in an atmosphere with an oxygen concentration of 50%.
168 hours for alkaline oxidative decomposition, followed by washing with water to remove alkaline components, then adding water to form a slurry, and wet pulverizing with a pearl mill (trade name) manufactured by Ashizawa Co., Ltd. A suspension was obtained. An aqueous solution of various concentrations of commercially available dextrin (manufactured by Matsutani Chemical Co., Ltd., trade name Paindex) was added and mixed as a dispersion aid to this aqueous suspension, and the concentration of the micronized cellulosic material was 5.0% by weight, and the concentration of dextrin 0. 05 wt%, 0.5 wt%, 2.0 wt%, 5.0 wt%, water 94.9 respectively
A mixture having a composition of 5% by weight, 94.5% by weight, 93% by weight and 90% by weight was obtained. The 50% cumulative volume particle size of the cellulosic materials in these mixtures was 1.7 μm, and the cumulative volume ratio of particles having a particle size of 3 μm or less was 72.1%. Next, these mixtures were put on a perforated plate, heated with stirring on a mantle heater to evaporate the water content, and the water removal was continued until the water content became 0.7 to 0.8 parts by weight. The redispersibility of the sludge-like compositions 1 to 4 of the present invention thus obtained in water was measured.

【0016】[0016]

【比較例1】実施例1〜4と同様の方法で、ただし、分
散補助剤を添加混合しないで、本発明外の組成物を得
た。実施例1〜4、及び比較例1の結果は表1に表わし
た。表1より、水分除去前の分散補助剤の有無にかかわ
らず、水への再分散性は強烈攪拌に施てはほとんど元の
分散状態へ戻ったが、本発明で重視する軽度攪拌の場合
は、分散補助剤0.01重量部以上の物と、分散補助剤
無しの物では大きな差異が見られた。
Comparative Example 1 A composition other than the present invention was obtained in the same manner as in Examples 1 to 4, but without adding and mixing a dispersion aid. The results of Examples 1 to 4 and Comparative Example 1 are shown in Table 1. From Table 1, regardless of the presence or absence of the dispersion aid before water removal, the redispersibility in water almost returned to the original dispersion state when subjected to intense stirring, but in the case of the mild stirring which is important in the present invention, A large difference was observed between the dispersion aid of 0.01 parts by weight or more and the product without the dispersion aid.

【0017】[0017]

【表1】 [Table 1]

【0018】[0018]

【実施例5〜7】実施例1〜4と同様の方法で得た水性
懸濁液に、分散補助剤としてキサンタンガム(三栄化学
製、商品名サンエース)の水溶液を添加混合し、微粒化
セルロース系素材濃度5.0重量%、キサンタンガム
0.05重量%、水94.95重量%の組成の混合物を
得た。この混合物を噴霧乾燥機で水分を蒸発除去してゆ
き、種々の含水率の本発明の含水組成物を得、これらの
組成物の水への再分散性を測定した。
[Examples 5 to 7] An aqueous suspension of xanthan gum (manufactured by San-ei Chemical Co., Ltd., trade name San-Ace) was added and mixed to an aqueous suspension obtained by the same method as in Examples 1 to 4 to form a finely divided cellulose-based composition. A mixture having a composition of a material concentration of 5.0% by weight, xanthan gum 0.05% by weight, and water 94.95% by weight was obtained. The water content of this mixture was removed by evaporation with a spray dryer to obtain water-containing compositions of the present invention having various water contents, and the redispersibility of these compositions in water was measured.

【0019】[0019]

【比較例2〜3】噴霧乾燥による水分蒸発除去を過度に
行い、0.17重量部を下廻る迄にした以外は実施例5
〜7と同一の方法で本発明外の組成物を得、これらの組
成物の水への再分散性を測定した。実施例5〜7、及び
比較例2〜3の結果は表2に表わした。
[Comparative Examples 2 to 3] Example 5 except that excessive evaporation of water by spray drying was performed and the amount was reduced to less than 0.17 parts by weight.
The compositions other than the present invention were obtained in the same manner as in ~ 7, and the redispersibility in water of these compositions was measured. The results of Examples 5-7 and Comparative Examples 2-3 are shown in Table 2.

【0020】[0020]

【表2】 [Table 2]

【0021】[0021]

【発明の効果】本発明の微粒化セルロース系素材の含水
組成物は、従来の懸濁液に比較して輸送に際して効率的
であり水分活性値の上昇により腐敗に対する抵抗性も小
さくなり、かつ水へ再分散させた時の分散性がすぐれて
おり通常の攪拌で容易に分散するので、ホモジナイザー
のような強烈攪拌による分散を必要としない。以上のご
とく、実用上使い勝手の良い供給形態を提供出来る。
INDUSTRIAL APPLICABILITY The water-containing composition of the micronized cellulosic material of the present invention is more efficient in transportation than conventional suspensions, and the resistance to rot is reduced due to the increase in water activity value, and Since it has excellent dispersibility when re-dispersed and is easily dispersed by ordinary stirring, it is not necessary to perform dispersion by vigorous stirring unlike a homogenizer. As described above, it is possible to provide a supply form that is practically easy to use.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 積算体積50%の粒径が0.3〜6μm
であり、かつ3μm以下の粒子の積算体積割合が25%
以上である微粒化セルロース系素材1重量部に対し水を
0.17〜3重量部、分散補助剤を0.01重量部以上
含有することを特徴とする微粒化セルロース系素材含水
組成物。
1. The particle size with an integrated volume of 50% is 0.3 to 6 μm.
And the cumulative volume ratio of particles of 3 μm or less is 25%
A water-containing composition of micronized cellulosic material, characterized by containing 0.17 to 3 parts by weight of water and 0.01 part by weight or more of a dispersion aid with respect to 1 part by weight of the above micronized cellulosic material.
JP22108892A 1992-08-20 1992-08-20 Micronized cellulose-based water-containing composition Expired - Fee Related JP3423334B2 (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004331918A (en) * 2003-05-12 2004-11-25 Asahi Kasei Chemicals Corp Amorphous cellulose fine powder
JP2009203559A (en) * 2008-02-26 2009-09-10 Daicel Chem Ind Ltd Fiber assembly of microfiber-shaped cellulose and method for producing the same
JP2014087313A (en) * 2012-10-31 2014-05-15 Asahi Kasei Chemicals Corp Confectionery including cellulose
JPWO2012111408A1 (en) * 2011-02-15 2014-07-03 日産化学工業株式会社 Fibrous resin reinforcing agent, method for producing the same, and resin composition using the same

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JPS59189141A (en) * 1983-03-28 1984-10-26 アイテイ−テイ−・インダストリ−ズ・インコ−ポレ−テツド Redispersible microfibrillated cellulose
JPS60186548A (en) * 1984-03-06 1985-09-24 Daicel Chem Ind Ltd Microfibrillated cellulose composition having excellent redispersing and suspending property
JPH02281050A (en) * 1989-04-21 1990-11-16 Agency Of Ind Science & Technol Novel water absorbing complex material and its production
JPH03163135A (en) * 1989-08-17 1991-07-15 Asahi Chem Ind Co Ltd Suspension of pulverized cellulosic material and its production
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US3827899A (en) * 1971-09-28 1974-08-06 For Ind Res Cir Ltd Centre Modified microcrystalline cellulose dispersion
JPS5455054A (en) * 1977-10-11 1979-05-01 Asahi Chem Ind Co Ltd Water-despersible compound
JPS59189141A (en) * 1983-03-28 1984-10-26 アイテイ−テイ−・インダストリ−ズ・インコ−ポレ−テツド Redispersible microfibrillated cellulose
JPS60186548A (en) * 1984-03-06 1985-09-24 Daicel Chem Ind Ltd Microfibrillated cellulose composition having excellent redispersing and suspending property
JPH02281050A (en) * 1989-04-21 1990-11-16 Agency Of Ind Science & Technol Novel water absorbing complex material and its production
JPH03163135A (en) * 1989-08-17 1991-07-15 Asahi Chem Ind Co Ltd Suspension of pulverized cellulosic material and its production
JP2944330B2 (en) * 1991-09-30 1999-09-06 旭化成工業株式会社 Water dispersible composite and its manufacturing method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004331918A (en) * 2003-05-12 2004-11-25 Asahi Kasei Chemicals Corp Amorphous cellulose fine powder
JP2009203559A (en) * 2008-02-26 2009-09-10 Daicel Chem Ind Ltd Fiber assembly of microfiber-shaped cellulose and method for producing the same
JPWO2012111408A1 (en) * 2011-02-15 2014-07-03 日産化学工業株式会社 Fibrous resin reinforcing agent, method for producing the same, and resin composition using the same
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JP2014087313A (en) * 2012-10-31 2014-05-15 Asahi Kasei Chemicals Corp Confectionery including cellulose

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