JPH03197501A - Disintegration of pulp sheet - Google Patents
Disintegration of pulp sheetInfo
- Publication number
- JPH03197501A JPH03197501A JP33760089A JP33760089A JPH03197501A JP H03197501 A JPH03197501 A JP H03197501A JP 33760089 A JP33760089 A JP 33760089A JP 33760089 A JP33760089 A JP 33760089A JP H03197501 A JPH03197501 A JP H03197501A
- Authority
- JP
- Japan
- Prior art keywords
- pulp
- water
- cellulose
- disintegrated
- crushing
- 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
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 12
- 230000009257 reactivity Effects 0.000 abstract description 10
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000006003 cornification Effects 0.000 abstract 1
- 229920002678 cellulose Polymers 0.000 description 19
- 239000001913 cellulose Substances 0.000 description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 16
- 239000002994 raw material Substances 0.000 description 14
- 229920002301 cellulose acetate Polymers 0.000 description 12
- 238000001914 filtration Methods 0.000 description 10
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 9
- 229960000583 acetic acid Drugs 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000006866 deterioration Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 230000003780 keratinization Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000006640 acetylation reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000001212 derivatisation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 2
- 229940069446 magnesium acetate Drugs 0.000 description 2
- 235000011285 magnesium acetate Nutrition 0.000 description 2
- 239000011654 magnesium acetate Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- -1 acetone Chemical compound 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、パルプシートの解砕方法に関し、詳しくはセ
ルロース誘導体の製造において、反応に先立って原料パ
ルプシートを解砕する際に、原料パルプシートを先ず水
中で解砕した後、解砕バルブ中の水を親水性有機溶剤で
置換し乾燥することにより、反応性に秀れた解砕パルプ
を乾燥状態で得る方法に関するものである。Detailed Description of the Invention (Industrial Application Field) The present invention relates to a method for crushing a pulp sheet, and more specifically, in the production of cellulose derivatives, when crushing a raw material pulp sheet prior to a reaction, the raw material pulp sheet is The present invention relates to a method of obtaining crushed pulp with excellent reactivity in a dry state by first crushing a sheet in water, replacing the water in the crushing valve with a hydrophilic organic solvent, and drying.
（従来の技術）
酢酸セルロース、硝酸セルロース、メチルセルロース、
エチルセルロース、ヒドロキシエチルセルロース、ヒド
ロキシプロピルセルロース、カルボキシメチルセルロー
スなどに代表されるセルロース誘導体の用途は衣料用繊
維、プラスチック、フィルム、フィルター素材、塗料、
インク、セラミックバインダー、食品添加剤など多岐に
わたり、工業的に重要なものである。(Prior art) Cellulose acetate, cellulose nitrate, methyl cellulose,
Cellulose derivatives such as ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, and carboxymethyl cellulose are used in clothing fibers, plastics, films, filter materials, paints,
It is industrially important in a wide variety of applications, including inks, ceramic binders, and food additives.
従来、セルロース誘導体の製造において、反応に先立っ
て乾燥状態で解砕されたセルロース原料を得る方法とし
て乾式解砕法が広く用いられて来た。乾式解砕法は、乾
燥状態（通常セルロースシートは乾燥状態で３〜１０％
程度の水分を含有する）の原料セルロースシートをその
ままアトリッションミル、ハンマーミル、カッターミル
などの乾式解砕機に供給し、解砕されたセルロース原料
を得る方法である。Conventionally, in the production of cellulose derivatives, a dry crushing method has been widely used as a method for obtaining cellulose raw materials that are crushed in a dry state prior to reaction. The dry crushing method is used in a dry state (usually cellulose sheets are 3 to 10%
In this method, a raw material cellulose sheet (containing a certain amount of water) is fed as it is to a dry crusher such as an attrition mill, hammer mill, or cutter mill to obtain a crushed cellulose raw material.
（発明が解決しようとする課題）
従来から、セルロース誘導体を製造する場合の原料セル
ロースとして、主としてαセルロース含有率の比較的高
いパルプか使用されて来た。(Problems to be Solved by the Invention) Conventionally, pulp with a relatively high α-cellulose content has been mainly used as the raw material cellulose for producing cellulose derivatives.
しかしながら、一般にセルロース原料は、世界的な資源
の制約とパルプ製造工場の公害聞届から要求価格に見合
う高品位のものは得られ難くなることが予想される。However, in general, it is expected that it will be difficult to obtain high-quality cellulose raw materials that meet the required price due to global resource constraints and pollution reports from pulp manufacturing plants.
αセルロース含有率の低い低品位パルプはその本来の使
用目的からパルプシートが固く、従来がら広く取り入れ
られている乾式解砕機では解砕効果が十分でなかったり
、また、解砕時の熱と衝撃により解砕物の反応性が著し
く劣化してしまい、誘導体化がうまく行えないことがし
ばしばある。Low-grade pulp with a low α-cellulose content has a hard pulp sheet due to its original purpose, and the conventionally widely used dry crusher does not have sufficient crushing effect, and the heat and shock during crushing As a result, the reactivity of the crushed material deteriorates significantly, and derivatization often cannot be carried out successfully.
原料セルロースシートを水中で解砕する方法は、乾式解
砕のように解砕時に熱や過度の衝撃を受けないため、解
砕時における反応性の劣化は少ないが、解砕後の含水状
態のパルプを常法にしたがって乾燥しようとすると、い
わゆる角質化が起り、反応性が著しく劣化してしまう。Unlike dry crushing, the method of crushing raw cellulose sheets in water does not subject them to heat or excessive shock during crushing, so there is little deterioration in reactivity during crushing, but the water content after crushing is If pulp is dried in a conventional manner, so-called keratinization occurs, resulting in a significant deterioration of reactivity.
このような現象を防ぐために、たとえば、酢酸セルロー
スの製造においては、原料セルロースシートを水中で解
砕し、反応溶媒である酢酸で解砕パルプ中の水を置換し
乾燥状態を経ずに反応に供する方法（米国特許第３７６
７１３４２号）があるが、この方法では乾燥状態で、反
応性に富んだ解砕されたセルロース原料を得ることはで
きない。多種多様なセルロース誘導体の製造のいずれに
も利用できるような解砕されたセルロース原料を、乾燥
状態で得る方法が必要とされている。In order to prevent this phenomenon, for example, in the production of cellulose acetate, the raw material cellulose sheet is crushed in water, and the water in the crushed pulp is replaced with acetic acid, which is a reaction solvent, so that the reaction can be carried out without going through a dry state. (U.S. Pat. No. 376)
No. 71342), but with this method it is not possible to obtain a highly reactive crushed cellulose raw material in a dry state. There is a need for a method of obtaining a crushed cellulose raw material in a dry state that can be used in the production of a wide variety of cellulose derivatives.
（課題を解決するための手段）
本発明者らは、解砕時の反応性劣化を防ぐため、原料セ
ルロースシートを水中で解砕することを前提とし、解砕
されたセルロース原料の乾燥時の角質化を防止し、かつ
乾燥性の良い親水性の置換用溶剤について、鋭意検討を
重ねた結果、本発明に到達したものである。(Means for Solving the Problems) In order to prevent reactivity deterioration during crushing, the present inventors assumed that the raw material cellulose sheet was crushed in water, and the The present invention was developed as a result of extensive research into hydrophilic replacement solvents that prevent keratinization and have good drying properties.
本発明は以下の方法によって実施される。The present invention is carried out by the following method.
まず、パルプシートを常法に従って水中で解砕し脱水す
る。脱水の方法としては、特に限定されないが、フィル
タープレスや遠心脱液が便利である。次に、得られた解
砕パルプのケーキ中に含ま一ル、イソプロパツールなど
の低級アルコール類や、アセトンなどのケトン類、テト
ラハイドロフランなどが上げられる。First, a pulp sheet is crushed and dehydrated in water according to a conventional method. The dehydration method is not particularly limited, but filter press and centrifugal dehydration are convenient. Next, lower alcohols such as alcohol and isopropanol, ketones such as acetone, and tetrahydrofuran are contained in the cake of the obtained crushed pulp.
置換に使用する親水性溶剤の量としては、使用する溶剤
の種類置換の方法によって異なるため限定できないが、
置換後のケーキ中の水分量を３０重量％（以下％はすべ
で重量％）以下にすることが必要である。置換後のケー
キ中の水分量が３０％を越えると乾燥時に角質化を起し
、反応性が劣ケーキ上に親水性溶剤をふりかける方法が
便利であり、工業的にも容易である。The amount of hydrophilic solvent used for substitution cannot be limited because it depends on the type of solvent used and the method of substitution.
It is necessary to reduce the water content in the cake after substitution to 30% by weight or less (hereinafter all percentages are % by weight). If the water content in the cake after substitution exceeds 30%, keratinization occurs during drying, and the reactivity is poor.A method of sprinkling a hydrophilic solvent on the cake is convenient and industrially easy.
次に、このようにして、水分量が３０％以下になるよう
に親水性溶剤で置換されたパルプケーキを脱液、乾燥し
、反応性に富んだ↓−−７状の解砕パルプを乾燥状態で
得るのであるが、パルプケーキをそのまま乾燥したので
は、パルプ間に再結合を□６、Ｗ状（７） ｔ＜ ／Ｌ
／プを得、。とができない。Next, the pulp cake, which has been replaced with a hydrophilic solvent so that the moisture content becomes 30% or less, is dehydrated and dried, and the highly reactive ↓-7-shaped crushed pulp is dried. However, if the pulp cake is dried as it is, the recombination between the pulps will occur □6, W-shaped (7) t< /L
/ Get a pu. I can't do it.
そこで、乾燥に先立って、あるいは、乾燥の途中で、未
乾燥状態あるいは乾燥途中の状態で、パルプケーキを再
解砕する必要がある。完全に乾燥し
さた後に再解砕を行うと乾式解砕と同じこととなり反応
性の劣化につながる。Therefore, it is necessary to re-crush the pulp cake prior to drying or during drying, either in an undried state or in a dry state. If re-crushing is performed after it is completely dry, it will be the same as dry crushing and lead to deterioration of reactivity.
本発明においては、パルプ中に揮発分（水分も含む、以
下同じ）が１０％以上残存している状態で再解砕を行う
。揮発分が１０％より少ない状態で再解砕を行うとセル
ロースの反応性が劣化する可能性が高い。In the present invention, re-crushing is performed in a state where 10% or more of volatile matter (including water, the same applies hereinafter) remains in the pulp. If re-crushing is performed in a state where the volatile content is less than 10%, there is a high possibility that the reactivity of cellulose will deteriorate.
再解砕の方法としては、特に限定されない。アトリッシ
ョンミル、ハンマーミル、カッターミル、ジェットミル
などが上げられるが、バルブケーキが特に柔らかい場合
は、圧搾空気を吹き付ける方法や振動を与える方法など
を採用することもできフラッフ
る。得られたχミヒ状パルプを常法に従って乾燥するこ
とにより、反応性に富んだ解砕パルプを乾燥状態で得る
ことができる。The re-crushing method is not particularly limited. Examples include attrition mills, hammer mills, cutter mills, jet mills, etc., but if the valve cake is particularly soft, methods such as blowing compressed air or applying vibration may also be used to fluff it. By drying the obtained χ-like pulp according to a conventional method, a highly reactive crushed pulp can be obtained in a dry state.
（発明の効果）
本発明の方法により、パルプシートから反応性フラ・ン
フ
の劣化をまねくことなく、チテ〒す状の解砕パルプを乾
燥状態で得ることができ、種々のセルロース誘導体の製
造において非常に有用である。特に、シートが硬いため
乾式解砕で利用が困難であった低グレードバルブを誘導
体化の原料として用いる場合に有用である。(Effects of the Invention) According to the method of the present invention, it is possible to obtain crushed pulp in the form of chunks in a dry state from a pulp sheet without causing deterioration of the reactive fluff, which is useful in the production of various cellulose derivatives. Very useful. It is particularly useful when using low-grade bulbs, which are difficult to use in dry crushing due to their hard sheets, as a raw material for derivatization.
（実施例）
以下に本発明を具体的に説明する実施例を示すが、本発
明は以下に示す実施例に限定されるものではない。(Examples) Examples are shown below to specifically explain the present invention, but the present invention is not limited to the examples shown below.
また、実施例中の部とは重量部を、％は重量％反応性を
評価するために、アセチル化反応を行い酢酸セルロース
を製造した。酢酸セルロースの製造は次の方法で行った
。Further, in the examples, "part" means "part by weight" and "%" means "wt%." In order to evaluate the reactivity, an acetylation reaction was carried out to produce cellulose acetate. Cellulose acetate was produced by the following method.
解砕バルブの水分を常法に従って、水分５％に調湿した
。この調湿バルブを前処理機に投入し、５％水分バルブ
１００部に対し、１００部の氷酢酸を均一に散布し４０
℃に３０分間混合しミ前処理活性化した。予め１２℃に
冷却した無水酢酸２５０部、酢酸３７５部、硫酸１．０
部の混液を捏和式酢化酸に準備しておき前記の前処理活
性化バルブを投入撹拌混合した。内容物は、原料バルブ
が同伴する水と無水酢酸との反応、及びセルロースと無
水酢酸との反応に依り、発熱するが初期の１６℃前後よ
り、６０分かけて７７℃に到達するように、外部冷却に
より調整し、さらに７７℃にて１２分間保持して酢化反
応行わせた。The moisture content of the crushing bulb was adjusted to 5% according to a conventional method. This humidity control valve was put into a pretreatment machine, and 100 parts of glacial acetic acid was evenly sprinkled on 100 parts of the 5% moisture valve.
℃ for 30 minutes to activate the pretreatment. 250 parts of acetic anhydride, 375 parts of acetic acid, and 1.0 parts of sulfuric acid cooled to 12°C in advance
A mixed solution of 1 part was prepared in a kneading type acetic acid, and the above-mentioned pretreatment activation valve was introduced and the mixture was stirred and mixed. The contents generate heat due to the reaction between the water entrained by the raw material valve and acetic anhydride, and the reaction between cellulose and acetic anhydride. The temperature was adjusted by external cooling, and the temperature was further maintained at 77° C. for 12 minutes to carry out the acetylation reaction.
次いで、１０部の２０％酢酸マグネシウム水溶液を添加
混合し、系内の硫酸を完全に中和し、且つ、酢酸マグネ
シウム過剰とした。完全中和したプ′
反応混合物をオートクレーブに移し、密閉下でゲラ０分
間保持した後、反応物を大気下に徐々にフラッシュさせ
て、反応混合物を１００℃とした。Next, 10 parts of a 20% aqueous magnesium acetate solution was added and mixed to completely neutralize the sulfuric acid in the system and make magnesium acetate excessive. The completely neutralized reaction mixture was transferred to an autoclave and kept under closed conditions for 0 minutes, and then the reaction mixture was gradually flushed to the atmosphere to bring the reaction mixture to 100°C.
反応混合物は激しい撹拌の下に、希酢酸水溶液を加えて
、フレーラス状酢酸セルロースとして分離した後、充分
水洗して取り出し乾燥した。A dilute aqueous acetic acid solution was added to the reaction mixture under vigorous stirring to separate it as a flared cellulose acetate, which was thoroughly washed with water, taken out and dried.
なお、原料パルプシートの密度はＪＩＳ Ｐ−８１１８
−１９７６により測定した。In addition, the density of the raw material pulp sheet is JIS P-8118.
-1976.
また、酢酸セルロース−物性測定は次の方法で粘 度：
酢酸セルロース濃度２０％になるよう９６％アセトン水
溶液に溶解し、２５±０．１’Ｃで、銅球（直径６，３
２關、重さ１．０４３ ｒ）が、酢酸セルロース溶液を
充たした内径２５．９ｍｍの管内を１０ｃｍ落下するに
要する時間（秒）
濾過量：９６％アセトン水溶液に２０部濃度に溶解した
酢酸セルロース溶液を５０℃で所定の濾布を通し、一定
圧力下に濾過する濾過量を測定し、次式により濾過量ｋ
Ｗを算出する。In addition, the physical properties of cellulose acetate can be measured using the following method:
Cellulose acetate was dissolved in a 96% acetone aqueous solution to a concentration of 20%, and heated at 25±0.1'C.
Time (seconds) required for a 25.9 mm inner diameter pipe (25.9 mm in diameter) to fall 10 cm through a tube filled with cellulose acetate solution. Amount of filtration: Cellulose acetate dissolved in a 96% acetone aqueous solution at a concentration of 20 parts. Pass the solution through a specified filter cloth at 50°C, measure the filtration amount under constant pressure, and calculate the filtration amount k using the following formula.
Calculate W.
Ｐｌ ：濾過開始から２０分間の濾過量（ｍｌ）Ｐ ：
２０分より６０分までの４０分間の濾過量（ｍｌ）
濾過量は、上記の式により算出できるが、これアセトン
溶液中の不溶解分の多少を表わしており、濾過量の悪い
酢酸セルロースは不溶解分が多いと考えられる。よって
、濾過量の悪い酢酸セルロースは当然紡糸ノズルへの閉
塞物も多くなり、糸切れ発生の度合いが増え、そのよう
な酢酸セルロースは可紡性が悪いと考えられる。そこで
、可紡性の評価として濾過量の測定結果で判定した。Pl: Filtration amount (ml) for 20 minutes from the start of filtration P:
Filtration amount (ml) for 40 minutes from 20 minutes to 60 minutes The filtration amount can be calculated using the above formula, but this represents the amount of insoluble matter in the acetone solution, and cellulose acetate, which has a poor filtration amount, is not It is thought that there is a large amount of dissolved matter. Therefore, cellulose acetate with a poor filtration rate naturally causes more obstructions to the spinning nozzle, increasing the occurrence of yarn breakage, and such cellulose acetate is considered to have poor spinnability. Therefore, the spinnability was evaluated based on the measurement results of the amount of filtration.
ここでいう可紡性とは、最高紡糸速度、ドラフト比、糸
切れ発生頻度が所定の基準値内に入ることを意味する。Spinnability here means that the maximum spinning speed, draft ratio, and yarn breakage frequency are within predetermined standard values.
実施例１〜６
表−１に記載した各種パルプシートのそれぞれについて
、２０ｇを水２Ｊ７を用いて、家庭用ミキサーで３０秒
間解砕し、ブフナーロートを用いて吸引脱水して、それ
ぞれ、含水バルブケーキ（Ａ）を得た。そのまま、ブフ
ナーロート上で（Ａ）に実施例１〜３では表−１に記載
した量のアセトンを、実施例４〜６ではイソプロパツー
ルをふりかけ、吸引脱液し、それぞれ溶剤置換バルブケ
ーキ（Ｂ）を得た。（Ｂ）に含まれる揮発分量と水分
０
量を表−１に示した。Examples 1 to 6 20g of each of the various pulp sheets listed in Table 1 was crushed using 2J7 water for 30 seconds in a household mixer, and dehydrated by suction using a Buchner funnel. A cake (A) was obtained. As it was, on a Buchner funnel, (A) was sprinkled with acetone in the amount shown in Table 1 for Examples 1 to 3, and isopropanol was sprinkled in Examples 4 to 6, and deliquified by suction to form a solvent displacement valve cake ( B) was obtained. Volatile content and moisture contained in (B)
0 amount is shown in Table-1.
次に、実施例１と２と４については（Ｂ）を室温で２時
間風乾した後、アトリッションミルで再解砕し、気流乾
燥機で乾燥して乾燥状態のフラッフ
タバルブを得た。また、実施例３と５と６については、
（Ｂ）をナイロン袋に投入し、第１図に示した方法で圧
搾空気を利用して再解砕し、気流乾各々の実施例におけ
る再解砕前のパルプケーキ中の揮発分を表−１に示した
。Next, for Examples 1, 2, and 4, (B) was air-dried at room temperature for 2 hours, crushed again in an attrition mill, and dried in a flash dryer to obtain a dry flutter valve. . Moreover, regarding Examples 3, 5, and 6,
(B) was put into a nylon bag, re-crushed using compressed air using the method shown in Fig. 1, and air-flow dried. Shown in 1.
フ 得られた、それぞれの乾燥フラッ久バルブを用った。centre Each of the obtained dried flash valves was used.
比較例１〜６
実施例１〜６と同じパルプシートをそのままアトリッシ
ョンミルで乾式解砕した。得られた解砕パルプは多くの
未解砕物を含んでいた。これらの解砕パルプを用いて、
実施例と同じ方法で酢酸セ１
４、Comparative Examples 1 to 6 The same pulp sheets as in Examples 1 to 6 were dry-pulverized as they were in an attrition mill. The obtained crushed pulp contained many uncrushed materials. Using these crushed pulp,
Acetic acid serum 14 in the same manner as in the examples,
第１図は、 本発明の実施例 （３゜ ５゜ ６） にお ける再解砕方法の説明図である。 Figure 1 shows Examples of the invention (3゜ 5゜ 6) Nii It is an explanatory view of the re-crushing method.
Claims (1)
親水性有機溶剤で置換した後乾燥することを特徴とする
パルプシートの解砕方法。A method for crushing a pulp sheet, which comprises crushing the pulp sheet in water, replacing the water in the crushed pulp with a hydrophilic organic solvent, and then drying the pulp sheet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33760089A JP2633042B2 (en) | 1989-12-26 | 1989-12-26 | Pulp sheet crushing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33760089A JP2633042B2 (en) | 1989-12-26 | 1989-12-26 | Pulp sheet crushing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03197501A true JPH03197501A (en) | 1991-08-28 |
| JP2633042B2 JP2633042B2 (en) | 1997-07-23 |
Family
ID=18310174
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33760089A Expired - Lifetime JP2633042B2 (en) | 1989-12-26 | 1989-12-26 | Pulp sheet crushing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2633042B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001354701A (en) * | 2000-06-14 | 2001-12-25 | Shin Etsu Chem Co Ltd | Method of manufacturing pulverized pulp and cellulose ether |
| JP4509454B2 (en) * | 2000-03-27 | 2010-07-21 | ダイセル化学工業株式会社 | Cellulose acetate and method for producing the same |
| WO2011111484A1 (en) * | 2010-03-09 | 2011-09-15 | コニカミノルタオプト株式会社 | Method for producing cellulose ester, cellulose ester, and cellulose ester film |
| EP3170843A4 (en) * | 2014-07-14 | 2017-09-13 | Daicel Corporation | Method for disintegrating pulp for cellulose acetate production, and process for producing cellulose acetate |
-
1989
- 1989-12-26 JP JP33760089A patent/JP2633042B2/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4509454B2 (en) * | 2000-03-27 | 2010-07-21 | ダイセル化学工業株式会社 | Cellulose acetate and method for producing the same |
| JP2010196056A (en) * | 2000-03-27 | 2010-09-09 | Daicel Chem Ind Ltd | Cellulose acetate and process for producing the same |
| JP2001354701A (en) * | 2000-06-14 | 2001-12-25 | Shin Etsu Chem Co Ltd | Method of manufacturing pulverized pulp and cellulose ether |
| WO2011111484A1 (en) * | 2010-03-09 | 2011-09-15 | コニカミノルタオプト株式会社 | Method for producing cellulose ester, cellulose ester, and cellulose ester film |
| JPWO2011111484A1 (en) * | 2010-03-09 | 2013-06-27 | コニカミノルタ株式会社 | Method for producing cellulose ester, cellulose ester, and cellulose ester film |
| EP3170843A4 (en) * | 2014-07-14 | 2017-09-13 | Daicel Corporation | Method for disintegrating pulp for cellulose acetate production, and process for producing cellulose acetate |
| US10954314B2 (en) | 2014-07-14 | 2021-03-23 | Daicel Corporation | Method of disintegrating pulp for use in cellulose acetate production and method of producing cellulose acetate |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2633042B2 (en) | 1997-07-23 |
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