JPH06206901A - Production of carboxymethyl cellulose having high bulk density - Google Patents

Production of carboxymethyl cellulose having high bulk density

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Publication number
JPH06206901A
JPH06206901A JP1945193A JP1945193A JPH06206901A JP H06206901 A JPH06206901 A JP H06206901A JP 1945193 A JP1945193 A JP 1945193A JP 1945193 A JP1945193 A JP 1945193A JP H06206901 A JPH06206901 A JP H06206901A
Authority
JP
Japan
Prior art keywords
cmc
bulk density
kneading
weight
residual solvent
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
JP1945193A
Other languages
Japanese (ja)
Other versions
JP2617410B2 (en
Inventor
Takayuki Sasaki
孝行 佐々木
Keiichi Takahashi
圭一 高橋
Shinji Miura
眞司 三浦
Nobuaki Fujioka
伸章 藤岡
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.)
Nippon Paper Industries Co Ltd
Jujo Paper Co Ltd
Original Assignee
Nippon Paper Industries Co Ltd
Jujo Paper 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 Nippon Paper Industries Co Ltd, Jujo Paper Co Ltd filed Critical Nippon Paper Industries Co Ltd
Priority to JP5019451A priority Critical patent/JP2617410B2/en
Publication of JPH06206901A publication Critical patent/JPH06206901A/en
Application granted granted Critical
Publication of JP2617410B2 publication Critical patent/JP2617410B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

PURPOSE:To produce carboxymethyl cellulose, having a high bulk density and excellent in powder fluidity without requiring regulation of the moisture content, etc., by kneading a reactional product etherified in a shearing apparatus according to a solvent method, then pulverizing the kneaded product and classifying the pulverized material. CONSTITUTION:A reactional product after completing the etherification according to a solvent method is kneaded in an apparatus to which a shearing force is applied, then dried, pulverized and classified to produce carboxymethyl cellulose having 600-950g/L bulk density. The water content in the amount of the residual solvent in the reactional product after the kneading is 80-99wt.%. The amount of the residual solvent before the kneading is 30-70wt.%. The bulk density is preferably 650-850g/L.

Description

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

【0001】[0001]

【産業上の利用分野】本発明は嵩密度が大で粉体流動性
に優れたカルボキシメチルセルロース(以下、CMCと
略す)の製造方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing carboxymethyl cellulose (hereinafter abbreviated as CMC) having a large bulk density and excellent powder fluidity.

【0002】[0002]

【従来の技術】CMCは、水溶性高分子電解質として増
粘剤、分散剤、保護コロイド剤、石油ボーリング用泥水
添加剤などとして広く一般に使用されている。その製造
方法は、溶媒法と水媒法に大別される。溶媒法に於いて
は、反応およびその後の精製工程で使用される有機溶媒
により、CMCは綿状となり易く、それを乾燥、粉砕、
分級したものの嵩密度は低くなり易く、包装材料費、輸
送運賃並びに倉庫保管料が割高となるなど好ましくな
い。また、一般に嵩密度の低い粉体は流動性が悪く、粉
体の取扱いが容易でない。そこで、これ等の欠点を解決
する目的で、CMCを顆粒状とする提案がなされ良好な
結果を収めている。
CMC is widely used as a water-soluble polymer electrolyte as a thickener, a dispersant, a protective colloid agent, a muddy water additive for petroleum boring and the like. The production method is roughly classified into a solvent method and an aqueous medium method. In the solvent method, CMC tends to be cotton-like due to the organic solvent used in the reaction and the subsequent purification step, and it is dried, crushed,
The bulk density of the classified product tends to be low, and the packaging material cost, the transportation freight charge, and the warehousing charge are unfavorably high. In addition, powders having a low bulk density generally have poor fluidity and are not easy to handle. Therefore, for the purpose of solving these drawbacks, a proposal has been made to make CMC into a granular form, and good results have been obtained.

【0003】CMCを顆粒状にする方法としては、予め
粉末状のCMCを特定の含水率に調整し、2本の相互に
反対方向に回転するロール間を通過させてフレーク状と
し、次いでこれを粉砕、分級する発明(特開昭54-16046
0)などがある。しかしながら、この方法によれば嵩密
度の高いCMCを得ることは可能であるが、フレーク化
する前に粉末状CMCを特定の含水率に調整しなければ
ならなかった。またCMCをフレーク状にする装置が必
要であるなど、工程およびその管理が煩雑となる欠点が
あった。
As a method for granulating CMC, powdered CMC is adjusted in advance to a specific water content, passed through two rolls rotating in mutually opposite directions to form flakes, which are then prepared. Invention of crushing and classifying (JP-A-54-16046)
0) etc. However, although it is possible to obtain CMC having a high bulk density by this method, it was necessary to adjust the powdery CMC to a specific water content before flake formation. Further, there is a drawback that the process and its management are complicated, for example, a device for making the CMC into a flake shape is required.

【0004】この欠点を改良した方法として特願平4-94
973が提案されている。即ち、未乾燥の未精製または精
製CMCを混練機に通した後、乾燥、粉砕、分級して得
ることを特徴とし、更に詳しくは未乾燥CMC中の残留
溶媒量を揮発分として30〜70重量%としたことを特徴と
する製造方法である。この方法では、CMCを混練機に
通すことによりCMCのゲル化が促進されるため、嵩密
度が向上した。しかし、この方法は有用であるが、混練
後のCMCの残留溶媒量中に占める水の割合が異なる場
合には安定した嵩密度の向上効果が充分に得られず、満
足する結果は得られていない。
As a method for improving this drawback, Japanese Patent Application No. 4-94
973 is proposed. That is, it is characterized in that it is obtained by passing undried unpurified or purified CMC through a kneader, then drying, pulverizing and classifying. More specifically, the residual solvent amount in the undried CMC is 30 to 70 wt% as volatile matter. % Is the manufacturing method. In this method, the gelation of CMC is promoted by passing the CMC through the kneader, so that the bulk density is improved. However, this method is useful, but when the proportion of water in the residual solvent amount of CMC after kneading is different, a stable effect of improving bulk density cannot be sufficiently obtained, and satisfactory results have been obtained. Absent.

【0005】[0005]

【発明が解決しようとする課題】本発明の目的は、せん
断力を与える装置を用いて、嵩密度が大きく、粉体流動
性にも優れたCMCを効率良く製造する方法を提供する
ことである。
SUMMARY OF THE INVENTION An object of the present invention is to provide a method for efficiently producing CMC having a large bulk density and excellent powder fluidity by using a device for applying a shearing force. .

【0006】[0006]

【課題を解決するための手段】本発明者等は、CMCの
混練条件と嵩密度の関係に就いて鋭意研究を重ねた結
果、CMCの残留溶媒量中に占める水の割合を特定の範
囲に調整しながら混練することにより、嵩密度と粉体流
動性を大きく向上できることを見出し、この知見に基づ
いて本発明を成すに至った。本発明は、溶媒法によりエ
ーテル化反応の終了した未精製または精製CMCをせん
断力の掛かる混練機で混練した後、乾燥、粉砕、分級す
ることにより達成される。本発明に於いて混練機で混練
した後のCMC中の残留溶媒量中に占める水の割合は80
〜98重量%で行なわれ、好ましくは85〜95重量%で行な
われる。このようにせん断力を与えた反応生成物の残留
溶媒量中の水を調整することにより、嵩密度が600〜950
g/L、好ましくは650〜850g/Lの粉末状CMCが効
率良く得られる。
Means for Solving the Problems As a result of intensive studies on the relationship between the kneading conditions of CMC and the bulk density, the present inventors have found that the proportion of water in the residual solvent amount of CMC falls within a specific range. It was found that bulk density and powder fluidity can be greatly improved by kneading while adjusting, and the present invention has been completed based on this finding. The present invention can be achieved by kneading unpurified or purified CMC which has been subjected to the etherification reaction by the solvent method with a kneader having a shearing force, followed by drying, pulverizing and classifying. In the present invention, the proportion of water in the residual solvent amount in CMC after kneading with a kneader is 80.
-98% by weight, preferably 85-95% by weight. By adjusting the amount of water in the residual solvent amount of the reaction product to which the shearing force is applied, the bulk density is 600 to 950.
The powdery CMC of g / L, preferably 650 to 850 g / L is efficiently obtained.

【0007】本発明記載の各測定値は以下の方法で行な
った。 残留溶媒量:110℃の送風乾燥器中に3時間放置し、元
の試料重量w1と放置後の試料重量w2とから次式により
求めた。 残留溶媒量中に占める水の割合:xgの試料に蒸留水30
gと1%セルラーゼ水溶液(商品名トリセラーゼ20、協
和発酵工業株式会社製)10gを加え24時間以上放置した
調製試料中の有機溶剤濃度(CMCの製造に使用した有
機溶剤類の総濃度)をガスクロマトグラフGC−7AG
(株式会社島津製作所)、カラム充填剤:商品名Por
apak Qで測定し、その値を使用して次式により求
めた。
Each measured value described in the present invention is measured by the following method.
It was. Residual solvent amount: left in a blast dryer at 110 ° C for 3 hours,
Sample weight w1And sample weight w after leaving2And from the following equation
I asked. Proportion of water in the amount of residual solvent: 30g of distilled water for xg sample
g and 1% cellulase aqueous solution (trade name Tricerase 20,
(Wako Hakko Kogyo Co., Ltd.) 10g was added and left for 24 hours or more
Concentration of organic solvent in prepared sample
Gas chromatograph GC-7AG
(Shimadzu Corporation), Column packing material: Product name Por
It is measured by apak Q and the value is used to obtain by the following equation.
I have

【0008】 本発明で使用することが出来る溶媒法によりエーテル化
反応の終了したCMCは、特に限定されるものではな
く、イソプロピルアルコール、エチルアルコール、メチ
ルアルコール、ベンゼンなどの有機溶剤の単独或いはそ
れ等の混合物と水とを反応媒体とし、セルロースにアル
カリの存在下でモノクロル酢酸などを作用させるなどの
公知の反応方法によって製造される。
[0008] The CMC which has been subjected to the etherification reaction by the solvent method that can be used in the present invention is not particularly limited, and may be an organic solvent such as isopropyl alcohol, ethyl alcohol, methyl alcohol or benzene alone or a mixture thereof. It is produced by a known reaction method in which water is used as a reaction medium and cellulose is allowed to act with monochloroacetic acid in the presence of an alkali.

【0009】本発明で効率良く得られる粉末状CMCの
嵩密度を600〜950g/L、好ましくは650〜850g/Lと
したのは、嵩密度が600g/L未満のものは本発明の製
造方法によらずとも容易に得られるためであり、好まし
くは650g/L以上のものを得る場合に適する。また、9
50g/L以上のCMCも得られるが効率良く得るために
は950g/L以下のもの、好ましくは850g/L以下のも
のを得る場合に適する。本発明で使用することが出来る
混練機は特に限定されるものではなく、被混練物に対し
てせん断力の掛かる混練機であれば公知の混練機を適宜
選択して使用することが出来るが、好ましくは2軸混練
機で温調装置が備わり、軸回転方向は原料投入口から見
てお互いに向かい合うもので且つ混練中に発生する気化
した有機溶媒などを捕集する機構を備えているものが望
ましい。
The powdery CMC efficiently obtained in the present invention has a bulk density of 600 to 950 g / L, preferably 650 to 850 g / L. This is because it can be easily obtained regardless of the method, and is preferably suitable for obtaining 650 g / L or more. Also, 9
Although CMC of 50 g / L or more can be obtained, it is suitable for obtaining 950 g / L or less, and preferably 850 g / L or less in order to obtain it efficiently. The kneading machine that can be used in the present invention is not particularly limited, and a known kneading machine can be appropriately selected and used as long as it is a kneading machine in which a shearing force is applied to the material to be kneaded, Preferably, it is a twin-screw kneader equipped with a temperature control device, the shaft rotation directions of which face each other as seen from the raw material inlet, and those equipped with a mechanism for collecting vaporized organic solvents generated during kneading. desirable.

【0010】本発明で混練した後のCMCの残留溶媒量
中に占める水の割合を80〜98重量%に、好ましくは85〜
95重量%になるようにするとしたのは、水の割合が80重
量%未満では得られる粉末状CMCの嵩密度と粉体流動
性の向上効果が充分に得られないためであり、好ましく
は85重量%以上が望ましい。また、残留溶媒中に占める
水の割合を98重量%以上としても嵩密度と粉体流動性は
大きく向上せず反ってCMCが一部糊状となり混練機の
内壁などに付着するなどの問題を生じるためであり、好
ましくは95重量%以下が望ましい。本発明では、混練し
た後のCMCの残留溶媒量中に占める有機溶剤量は2〜
20重量%となるが、有機溶剤がイソプロピルアルコール
の場合にはそれが全有機剤中の10重量%以上となること
が好ましい。混練する前のCMCの残留溶媒量が30重量
%未満では混練機には過大な負荷が掛かり安定的に混練
機を運転することが困難となり、70重量%超では混練機
でCMCの残留揮発分中に占める水の割合を目的とする
範囲に効率良く調整出来ず、嵩密度および粉体流動性改
善効果の発現性が良好でないため好ましくない。
The proportion of water in the residual solvent amount of CMC after kneading in the present invention is 80 to 98% by weight, preferably 85 to 98% by weight.
The reason why the amount of water is set to 95% by weight is that if the proportion of water is less than 80% by weight, the effect of improving the bulk density and the powder fluidity of the obtained powdery CMC cannot be sufficiently obtained. Weight% or more is desirable. Also, even if the proportion of water in the residual solvent is 98% by weight or more, the bulk density and powder fluidity are not significantly improved, and there is a problem that CMC partially becomes pasty and adheres to the inner wall of the kneader. This is because it occurs, and it is preferably 95% by weight or less. In the present invention, the amount of organic solvent in the residual solvent amount of CMC after kneading is 2 to
It is 20% by weight, but when the organic solvent is isopropyl alcohol, it is preferably 10% by weight or more in the total organic agent. If the residual solvent content of CMC before kneading is less than 30% by weight, the kneading machine will be overloaded and it will be difficult to operate the kneading machine stably. If it exceeds 70% by weight, the residual volatile content of CMC in the kneading machine will be high. It is not preferable because the proportion of water in the water cannot be efficiently adjusted to a target range, and the bulk density and the powder fluidity improving effect are not well expressed.

【0011】[0011]

【実施例】以下に本発明に就いて更に詳述するが、本発
明はこれによって限定されるものではない。
The present invention will be described in more detail below, but the present invention is not limited thereto.

【0012】実施例1 容量5Lの2軸ニーダにイソプロピルアルコール1526g
と水酸化ナトリウム96.4gを水248gに溶解したものを
添加する。温度を25℃に保ちながらリンターパルプ214
gを投入する。この温度を保ちながら90分間撹拌、混合
してアルセル反応を行なわせた。次いで、モノクロル酢
酸108.5gを90%イソプロピルアルコール200gに溶解し
たものを加え、この温度で30分間保持した後、30分を要
して70℃まで昇温し、この温度で60分間エーテル化反応
を行なわせた。エーテル化終了後、酢酸で中和し、75重
量%のメチルアルコール10Lで2回精製し、遠心脱水
機で脱液して残留溶媒量が50.3重量%のCMCを得た。
Example 1 1526 g of isopropyl alcohol was added to a biaxial kneader having a volume of 5 L.
And 96.4 g of sodium hydroxide dissolved in 248 g of water are added. Linter pulp 214 while keeping the temperature at 25 ℃
Add g. While maintaining this temperature, the mixture was stirred and mixed for 90 minutes to carry out the Alcel reaction. Next, 108.5 g of monochloroacetic acid dissolved in 200 g of 90% isopropyl alcohol was added, and after holding at this temperature for 30 minutes, the temperature was raised to 70 ° C over 30 minutes, and the etherification reaction was performed at this temperature for 60 minutes. I did it. After completion of the etherification, the mixture was neutralized with acetic acid, purified twice with 10 L of 75% by weight methyl alcohol, and deliquored with a centrifugal dehydrator to obtain CMC having a residual solvent amount of 50.3% by weight.

【0013】更に、得られたCMCをジャケット式温調
装置が備わり、お互いに向かいあう方向に100rpmで回転
している2軸混練機(歯とケーシングのクリアランス2.
0mm)に500g投入して10分間混練した。混練中ジャケッ
ト式温調装置には81℃の熱媒体を循環させた。混練後の
CMCの中の残留溶媒量中に占める水の割合は82.3重量
%であった。次いでこのCMCを乾燥、粉砕して粉末状
CMCとした。
Further, the obtained CMC is equipped with a jacket type temperature controller, and is a twin-screw kneader rotating at 100 rpm in a direction facing each other (clearance between teeth and casing 2.
(0 mm) and kneaded for 10 minutes. During the kneading, a heating medium of 81 ° C was circulated in the jacket type temperature controller. The proportion of water in the residual solvent amount in the CMC after kneading was 82.3% by weight. Next, this CMC was dried and pulverized to obtain powdered CMC.

【0014】実施例2 実施例1と全く同様の処方、手順で反応、精製、脱液し
た残留溶媒量が50.8重量%のCMCを実施例1と全く同
様の2軸混練機に500g投入して10分間混練した。混練
中ジャケット式温調装置には65℃の熱媒体を循環させ
た。混練機のCMC中の残留溶媒量中に占める水の割合
は81.2重量%であった。次いでこのCMCを乾燥、粉砕
して粉末状CMCとした。
Example 2 500 g of CMC having a residual solvent amount of 50.8% by weight, which had been reacted, purified and deliquored by the same formulation and procedure as in Example 1, was charged into the same biaxial kneader as in Example 1 by 500 g. Kneaded for 10 minutes. During the kneading, a heating medium of 65 ° C was circulated through the jacket type temperature controller. The proportion of water in the residual solvent amount in the CMC of the kneader was 81.2% by weight. Next, this CMC was dried and pulverized to obtain powdered CMC.

【0015】実施例3 実施例1と全く同様の処方、手順で反応、精製、脱液し
た残留溶媒量が50.1重量%のCMCを実施例1と全く同
様の2軸混練機に500g投入して10分間混練した。混練
中ジャケット式温調装置には98℃の熱媒体を循環させ
た。混練後のCMC中の残留溶媒量中に占める水の割合
は96.3重量%であった。次いでこのCMCを乾燥、粉砕
して粉末状CMCとした。
Example 3 500 g of CMC having a residual solvent amount of 50.1% by weight, which had been reacted, purified and deliquored by the same formulation and procedure as in Example 1, was charged in the same twin-screw kneader as in Example 1. Kneaded for 10 minutes. During the kneading, a heating medium of 98 ° C was circulated in the jacket type temperature controller. The proportion of water in the residual solvent amount in the CMC after kneading was 96.3% by weight. Next, this CMC was dried and pulverized to obtain powdered CMC.

【0016】比較例1 実施例1と全く同様の処方、手順で反応、精製、脱液し
た残留溶媒量が50.7重量%のCMCを実施例1と全く同
様の2軸混練機に500g投入して10分間混練した。混練
中ジャケット式温調装置には20℃の水を循環させた。混
練後のCMC中の残留溶媒量中に占める水の割合は67.3
重量%であった。次いでこのCMCを乾燥、粉砕して粉
末状CMCとした。
Comparative Example 1 500 g of a CMC having a residual solvent amount of 50.7% by weight, which had been reacted, purified and deliquored by the same formulation and procedure as in Example 1, was placed in the same biaxial kneader as in Example 1 (500 g). Kneaded for 10 minutes. During the kneading, water at 20 ° C was circulated in the jacket type temperature controller. The ratio of water in the residual solvent amount in CMC after kneading is 67.3.
% By weight. Next, this CMC was dried and pulverized to obtain powdered CMC.

【0017】比較例2 実施例1と全く同様の処方、手順で反応、精製、脱液し
た残留溶媒量が50.2重量%のCMCを実施例1と全く同
様の2軸混練機に500g投入して10分間混練した。混練
中ジャケット式温調装置には50℃の熱媒体を循環させ
た。混練機のCMC中の残留溶媒量中に占める水の割合
は70.5重量%であった。次いでこのCMCを乾燥、粉砕
して粉末状CMCとした。
Comparative Example 2 500 g of CMC having a residual solvent amount of 50.2% by weight which had been reacted, purified and deliquored by the same formulation and procedure as in Example 1 was charged into the same twin-screw kneader as in Example 1. Kneaded for 10 minutes. During the kneading, a heating medium of 50 ° C was circulated in the jacket-type temperature controller. The proportion of water in the residual solvent amount in the CMC of the kneader was 70.5% by weight. Next, this CMC was dried and pulverized to obtain powdered CMC.

【0018】比較例3 実施例1と全く同様の処方、手順で反応、精製、脱液し
た残留溶媒量が50.8重量%のCMCを実施例1と全く同
様の2軸混練機に500g投入して10分間混練した。混練
中ジャケット式温調装置には105℃の熱媒体を循環させ
た。混練は問題なく行なえたが、CMCの糊化したもの
が混練機の内壁に付着していたため、それを除去するた
めに時間を要し作業性が悪かった。混練機のCMC中の
残留溶媒量中に占める水の割合は98.5重量%であった。
次いでこのCMCを乾燥、粉砕して粉末状CMCとし
た。
Comparative Example 3 500 g of CMC having a residual solvent amount of 50.8% by weight which had been reacted, purified and deliquored by the same formulation and procedure as in Example 1 was charged into the same twin-screw kneader as in Example 1. Kneaded for 10 minutes. During the kneading, a heating medium of 105 ° C was circulated in the jacket type temperature controller. The kneading could be performed without any problem, but the gelatinized CMC adhered to the inner wall of the kneading machine, and it took time to remove it and the workability was poor. The proportion of water in the residual solvent amount in the CMC of the kneader was 98.5% by weight.
Next, this CMC was dried and pulverized to obtain powdered CMC.

【0019】比較例4 実施例1と全く同様の処方、手順で反応、精製して充分
に脱液した残留溶媒量が28.0重量%となるCMCを実施
例1と全く同様の2軸混練機に500g投入して混練した
が混練機の負荷が急激に上昇したため、混練機の運転を
中止した。
Comparative Example 4 CMC having a residual solvent amount of 28.0% by weight, which had been reacted and purified by the same formulation and procedure as in Example 1 and had been sufficiently deliquored, was placed in the same twin-screw kneader as in Example 1. Although 500 g was added and kneaded, the load on the kneader increased rapidly, so the operation of the kneader was stopped.

【0020】比較例5 実施例1と全く同様の処方、手順で反応、精製、脱液し
て残留溶媒量が74.0重量%となるCMCを実施例1と全
く同様の2軸混練機に500g投入して10分間混練した。
混練中ジャケット式温調装置には81℃の熱媒体を循環さ
せた。混練機のCMC中の残留溶媒量中に占める水の割
合は60.2重量%であった。次いでこのCMCを乾燥、粉
砕して粉末状CMCとした。
Comparative Example 5 CMC having a residual solvent amount of 74.0% by weight after reaction, purification and deliquoring in exactly the same formulation and procedure as in Example 1 was charged to the same biaxial kneader as in Example 1 (500 g). And kneaded for 10 minutes.
During the kneading, a heating medium of 81 ° C was circulated in the jacket type temperature controller. The proportion of water in the amount of residual solvent in the CMC of the kneader was 60.2% by weight. Next, this CMC was dried and pulverized to obtain powdered CMC.

【0021】以上の実施例1〜3および比較例1〜3,
5で得た粉末状CMCの性状を表1に示した。表1に示
されるように、CMCを混練機で混練し混練後のCMC
中の残留溶媒量中に占める水の割合を特定の範囲に調整
することにより、得られるCMCの嵩密度と粉体流動性
が大きく向上することが実証された。
The above Examples 1-3 and Comparative Examples 1-3,
The properties of the powdered CMC obtained in No. 5 are shown in Table 1. As shown in Table 1, CMC is kneaded by a kneader and kneaded.
It was demonstrated that the bulk density and powder fluidity of the obtained CMC were significantly improved by adjusting the proportion of water in the residual solvent amount in the specific range.

【0022】[0022]

【表1】 [Table 1]

【0023】*1;50ccのメスシリンダーに粉末状CM
Cを10g入れ高さ3cmのところから数回落下させ、容量
が変化しなくなった時点での容量を測定し、その測定値
から嵩密度を計算した。 *2;直径8cmの円板上にロートを介して粉末状CMC
を注入して形成された円錐状の堆積層の角度を分度器を
用いて測定した値。
* 1: Powder CM in a 50cc measuring cylinder
10 g of C was dropped and dropped several times from a height of 3 cm, and the volume was measured when the volume stopped changing, and the bulk density was calculated from the measured value. * 2: Powdered CMC through a funnel on a disk with a diameter of 8 cm
A value obtained by measuring the angle of the conical sedimentary layer formed by injecting the liquid using a protractor.

【0024】[0024]

【発明の効果】以上詳述した如く、本発明の製造方法に
よると、溶媒法によりエーテル化の終了したCMCをせ
ん断力の掛かる混練機で混練することにより容易に粉末
状CMCの嵩密度と粉体流動性を大きくすることが出
来、従来のようにCMCを顆粒状とすることもなく粉末
状のままでも嵩密度と粉体流動性が改善される。それに
よりCMCの顆粒状化のために必要であった、予め粉砕
されたCMCの特定の含水率への調整やCMCをフレー
ク状にする装置が不要となる。更に効率良く嵩密度と粉
体流動性の大きいCMCが得られるなど、本製造方法の
もたらすメリットは大きい。
As described in detail above, according to the production method of the present invention, the bulk density and powder of CMC powder can be easily obtained by kneading the CMC which has been etherified by the solvent method with a kneader to which a shearing force is applied. The body fluidity can be increased, and the bulk density and the powder fluidity can be improved even when the CMC is not in the granular form as in the conventional case but is in the powder form. This eliminates the need for adjusting the pre-ground CMC to a specific water content and the device for flaking the CMC, which was necessary for granulating the CMC. Further, the merits brought about by the present production method are great, such as the CMC having high bulk density and powder fluidity can be obtained more efficiently.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 溶媒法によりエーテル化が終了した反応
生成物を、せん断力の掛かる装置で混練した後、乾燥、
粉砕、分級して得ることを特徴とする嵩密度が600〜950
g/Lのカルボキシメチルセルロースの製造方法。
1. The reaction product, which has been etherified by the solvent method, is kneaded in a device to which a shearing force is applied, and then dried,
Bulk density of 600 to 950, which is characterized by being crushed and classified
A method for producing g / L carboxymethyl cellulose.
【請求項2】 混練後の反応生成物の残留溶媒量中に占
める水の割合を80〜98重量%にすることを特徴とする請
求項1に記載のカルボキシメチルセルロースの製造方
法。
2. The method for producing carboxymethyl cellulose according to claim 1, wherein the proportion of water in the residual solvent amount of the reaction product after kneading is 80 to 98% by weight.
【請求項3】 混練前の反応生成物中の残留溶媒量が、
30〜70重量%であることを特徴とする請求項1または2
に記載のカルボキシメチルセルロースの製造方法。
3. The amount of residual solvent in the reaction product before kneading is
30 to 70% by weight of claim 1 or 2 characterized in that
The method for producing carboxymethyl cellulose according to 1.
JP5019451A 1993-01-13 1993-01-13 Method for producing carboxymethyl cellulose having high bulk density Expired - Fee Related JP2617410B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5019451A JP2617410B2 (en) 1993-01-13 1993-01-13 Method for producing carboxymethyl cellulose having high bulk density

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5019451A JP2617410B2 (en) 1993-01-13 1993-01-13 Method for producing carboxymethyl cellulose having high bulk density

Publications (2)

Publication Number Publication Date
JPH06206901A true JPH06206901A (en) 1994-07-26
JP2617410B2 JP2617410B2 (en) 1997-06-04

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ID=11999683

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Country Link
JP (1) JP2617410B2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001520281A (en) * 1997-10-20 2001-10-30 ヴオルフ・ヴアルスロデ・アクチエンゲゼルシヤフト Substantially fiber-free cellulose ethers exhibiting improved water retention, methods of making and using the same
JP2001302701A (en) * 2000-02-15 2001-10-31 Shin Etsu Chem Co Ltd Preparation method of alkali cellulose and cellulose ether
WO2010117781A1 (en) * 2009-03-31 2010-10-14 Dow Global Technologies Inc. Carboxymethyl cellulose with improved properties

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001520281A (en) * 1997-10-20 2001-10-30 ヴオルフ・ヴアルスロデ・アクチエンゲゼルシヤフト Substantially fiber-free cellulose ethers exhibiting improved water retention, methods of making and using the same
JP2001302701A (en) * 2000-02-15 2001-10-31 Shin Etsu Chem Co Ltd Preparation method of alkali cellulose and cellulose ether
WO2010117781A1 (en) * 2009-03-31 2010-10-14 Dow Global Technologies Inc. Carboxymethyl cellulose with improved properties
JP2012521785A (en) * 2009-03-31 2012-09-20 ダウ グローバル テクノロジーズ エルエルシー Tartrate stabilizer for wine

Also Published As

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