JP2020012021A - 繊維状セルロース含有物及びその製造方法、繊維状セルロース乾燥体及びその製造方法、並びに繊維状セルロース複合樹脂及びその製造方法 - Google Patents
繊維状セルロース含有物及びその製造方法、繊維状セルロース乾燥体及びその製造方法、並びに繊維状セルロース複合樹脂及びその製造方法 Download PDFInfo
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- JP2020012021A JP2020012021A JP2018133240A JP2018133240A JP2020012021A JP 2020012021 A JP2020012021 A JP 2020012021A JP 2018133240 A JP2018133240 A JP 2018133240A JP 2018133240 A JP2018133240 A JP 2018133240A JP 2020012021 A JP2020012021 A JP 2020012021A
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- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
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- 125000005498 phthalate group Chemical class 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
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- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- ZNZJJSYHZBXQSM-UHFFFAOYSA-N propane-2,2-diamine Chemical compound CC(C)(N)N ZNZJJSYHZBXQSM-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- PBMFSQRYOILNGV-UHFFFAOYSA-N pyridazine Chemical compound C1=CC=NN=C1 PBMFSQRYOILNGV-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- SBYHFKPVCBCYGV-UHFFFAOYSA-N quinuclidine Chemical compound C1CC2CCN1CC2 SBYHFKPVCBCYGV-UHFFFAOYSA-N 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 150000003330 sebacic acids Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- IZUPJOYPPLEPGM-UHFFFAOYSA-M sodium;hydron;phthalate Chemical compound [Na+].OC(=O)C1=CC=CC=C1C([O-])=O IZUPJOYPPLEPGM-UHFFFAOYSA-M 0.000 description 1
- 229940063673 spermidine Drugs 0.000 description 1
- 229940063675 spermine Drugs 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 235000011044 succinic acid Nutrition 0.000 description 1
- 150000003444 succinic acids Chemical class 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- YSGSDAIMSCVPHG-UHFFFAOYSA-N valyl-methionine Chemical compound CSCCC(C(O)=O)NC(=O)C(N)C(C)C YSGSDAIMSCVPHG-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
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- C08L1/02—Cellulose; Modified cellulose
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- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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- C08B3/12—Preparation of cellulose esters of organic acids of polybasic organic acids
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- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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Abstract
Description
平均繊維幅0.1μm以上のマイクロ繊維セルロースと、平均粒子径1〜1500μmの樹脂粉末とを含む、
ことを特徴とする繊維状セルロース含有物。
前記マイクロ繊維セルロース100質量部に対する前記樹脂粉末の配合割合が、10〜100000質量部である、
請求項1に記載の繊維状セルロース含有物。
前記マイクロ繊維セルロースは、平均繊維長0.02〜3.0mm、フィブリル化率1.0%以上である、
請求項1又は請求項2に記載の繊維状セルロース含有物。
前記マイクロ繊維セルロースが多塩基酸で変性されており、及び/又は、
前記繊維状セルロース含有物が多塩基酸を含む、
請求項1〜3のいずれか1項に記載の繊維状セルロース含有物。
平均繊維幅0.1μm以上のマイクロ繊維セルロースと、平均粒子径1〜1500μmの樹脂粉末とを含む繊維状セルロース含有物が乾燥されてなる、
ことを特徴とする繊維状セルロース乾燥体。
平均繊維幅0.1μm以上のマイクロ繊維セルロースと、平均粒子径1〜1500μmの樹脂粉末とを含む繊維状セルロース含有物の乾燥体が混練されてなる、
ことを特徴とする繊維状セルロース複合樹脂。
原料パルプを平均繊維幅が0.1μm以上に留まる範囲で解繊してマイクロ繊維セルロースの分散液を得、
この分散液と平均粒子径1〜1500μmの樹脂粉末とを混合する、
ことを特徴とする繊維状セルロース含有物の製造方法。
原料パルプを平均繊維幅が0.1μm以上に留まる範囲で解繊してマイクロ繊維セルロースの分散液を得、
この分散液と平均粒子径1〜1500μmの樹脂粉末とを混合して繊維状セルロース含有物を得、
この繊維状セルロース含有物を、含水率が95%以下となるように濃縮したうえで乾燥する、
ことを特徴とする繊維状セルロース乾燥体の製造方法。
原料パルプを平均繊維幅が0.1μm以上に留まる範囲で解繊してマイクロ繊維セルロースの分散液を得、
この分散液と平均粒子径1〜1500μmの樹脂粉末とを混合して繊維状セルロース含有物を得、
この繊維状セルロース含有物を乾燥して繊維状セルロース乾燥体を得、
この繊維状セルロース乾燥体を混練する、
ことを特徴とする繊維状セルロース複合樹脂の製造方法。
前記繊維状セルロース乾燥体と樹脂ペレットとを混練するものとし、
前記繊維状セルロース乾燥体は、前記マイクロ繊維セルロース100質量部に対して樹脂粉末が10000質量部以下の配合割合で含まれるものとし、
前記樹脂粉末100質量部に対する前記樹脂ペレットの配合割合を10〜100000質量部とする、
請求項9に記載の繊維状セルロース複合樹脂の製造方法。
平均繊維幅0.1μm以上のマイクロ繊維セルロースは、原料繊維(パルプ繊維)を微細化(解繊)処理して得ることができる。原料となる繊維としては、植物由来の繊維、動物由来の繊維、微生物由来の繊維等の中から1種又は2種以上を選択して使用することができる。ただし、植物繊維であるパルプ繊維を使用するのが好ましい。原料繊維がパルプ繊維であると、安価であり、また、サーマルリサイクルの問題を避けることができる。
原料繊維は、解繊に先立って化学的手法によって前処理するのが好ましい。微細化処理(解繊)に先立って化学的手法によって前処理することで、微細化処理の回数を大幅に減らすことができ、微細化処理のエネルギーを大幅に削減することができる。
原料繊維の微細化処理は、例えば、ビーター、高圧ホモジナイザー、高圧均質化装置等のホモジナイザー、グラインダー、摩砕機等の石臼式摩擦機、単軸混練機、多軸混練機、ニーダーリファイナー等を使用して原料繊維を叩解することによって行うことができる。ただし、微細化処理は、リファイナーを使用して行うのが好ましい。
微細化処理して得られたマイクロ繊維セルロースは、水系媒体中に分散して分散液とする。水系媒体は、全量が水であるのが特に好ましいが、一部が水と相溶性を有する他の液体である水系媒体も好ましく使用することができる。他の液体としては、炭素数3以下の低級アルコール類等を使用することができる。
次に、マイクロ繊維セルロース分散液は、平均粒子径1〜1500μmの樹脂粉末と混合する。樹脂粉末を混合すると、次いで脱水・乾燥したマイクロ繊維セルロース同士の水素結合が阻害され、分散性が向上する。また、マイクロ繊維セルロースの平均繊維径が0.1μm以上であることと相まって脱水が可能になり、乾燥のエネルギーを大きく減らすことができる。したがって、樹脂粉末の添加は、前述した分散液の濃縮に際して行うこともできる。
マイクロ繊維セルロース及び樹脂粉末を含む繊維状セルロース含有物は、乾燥して、好ましくは脱水及び乾燥して繊維状セルロース乾燥体にする。本形態の繊維状セルロース含有物は、セルロースナノファイバーではなくマイクロ繊維セルロースを含んでいるので脱水することができる。しかも、本形態の繊維状セルロース含有物は、樹脂粉末を含んでいるので脱水を容易に行うことができる。乾燥に先立って脱水しておけば、乾燥に要するエネルギーが極めて小さなものとなる。また、樹脂粉末を含んでいるので、繊維状セルロース含有物を繊維状セルロース乾燥体としても分散しなくなる可能性が低い。
繊維状セルロース乾燥体は、必要により樹脂ペレットを添加して混練し、もって繊維状セルロース複合樹脂とする。なお、樹脂ペレットを添加しない場合は、単に熱を加える等して混練することで、繊維状セルロース乾燥体が繊維状セルロース複合樹脂になる。なお、前述したとおり、本形態における樹脂ペレットの種類等に関する説明は、前述した樹脂粉末にも該当する。
ここで多塩基酸について説明を加える。
マイクロ繊維セルロースを変性する場合、その方法としては、例えば、エステル化、エーテル化、アミド化、スルフィド化等の疎水変性を挙げることができる。ただし、マイクロ繊維セルロースを疎水変性する方法としては、エステル化を採用するのが好ましい。
マイクロ繊維セルロースには、セルロースナノファイバー、ミクロフィブリルセルロース、ミクロフィブリル状微細繊維、微少繊維セルロース、ミクロフィブリル化セルロース、スーパーミクロフィブリルセルロース等と称される各種微細繊維の中から1種又は2種以上を含ませることができ、また、これらの微細繊維が含まれていてもよい。また、これらの微細繊維を更に微細化した繊維をも含ませることもでき、また、含まれていてもよい。ただし、全原料繊維中におけるマイクロ繊維セルロースの割合が10質量%以上、好ましくは30質量%以上、より好ましくは60質量%以上となるようにする必要がある。
繊維状セルロース乾燥体及び樹脂ペレットの混練物は、必要により再度混練処理を行った後、所望の形状に成形して繊維状セルロース複合樹脂とすることもできる。なお、混練物に変性マイクロ繊維セルロースが分散していても、成形加工性に優れている。
明細書中の用語は、特に断りのない限り、以下のとおりである。
固形分濃度0.01〜0.1質量%のマイクロ繊維セルロースの水分散液100mlをテフロン(登録商標)製メンブレンフィルターでろ過し、エタノール100mlで1回、t−ブタノール20mlで3回溶媒置換する。次に、凍結乾燥し、オスミウムコーティングして試料とする。この試料について、構成する繊維の幅に応じて5000倍、10000倍又は30000倍のいずれかの倍率で電子顕微鏡SEM画像による観察を行う。具体的には、観察画像に二本の対角線を引き、対角線の交点を通過する直線を任意に三本引く。さらに、この三本の直線と交錯する合計100本の繊維の幅を目視で計測する。そして、計測値の中位径を平均繊維径とする。
平均繊維長とフィブリル化率は、バルメット社製の繊維分析計「FS5」によって測定する。
上記平均繊維長を平均繊維幅(径)で除した値である。
JIS−K0131(1996)の「X線回折分析通則」に準拠して、X線回折法により測定した値である。なお、マイクロ繊維セルロースは、非晶質部分と結晶質部分とを有し、結晶化度は、マイクロ繊維セルロース全体における結晶質部分の割合を意味することになる。
JIS−P8215(1998)に準拠して測定する。なお、パルプ粘度が高いほどマイクロ繊維セルロースの重合度が高いことを意味する。
JIS P8121−2:2012に準拠して測定した値である。
繊維の水分率は、定温乾燥機を用いて、試料を105℃で6時間以上保持し質量の変動が認められなくなった時点の質量を乾燥後質量とし、下記式にて算出した値である。
繊維水分率(%)=[(乾燥前質量−乾燥後質量)÷乾燥前質量]×100
固形分濃度2.75重量%のマイクロ繊維セルロース水分散液365gに、ポリプロピレン樹脂粉末83gを添加し、No.2ろ紙にて30分間吸引濾過して脱水して繊維状セルロース含有物を得た。
曲げ弾性率は、JIS K7171:2008に準拠して測定した。表中には、評価結果を以下の基準で示した。
樹脂自体の曲げ弾性率を1として複合樹脂の曲げ弾性率(倍率)が1.5倍以上の場合 :○
樹脂自体の曲げ弾性率を1として複合樹脂の曲げ弾性率(倍率)が1.5倍未満の場合:×
表1に示すように、各種条件を変化させて実施例1と同様の試験を行った。結果は、表1に示した。なお、多塩基酸は基本的に混練直前に添加することとした。
固形分濃度2.75重量%のマイクロ繊維セルロース水分散液365gに、ポリプロピレン樹脂粉末10gを添加し、No.2ろ紙にて30分間吸引濾過して脱水して繊維状セルロース含有物を得た。
表2に示すように、各種条件を変化させて実施例7と同様の試験を行った。結果は、表2に示した。なお、多塩基酸は基本的に混練直前に添加することとした。
Claims (10)
- 平均繊維幅0.1μm以上のマイクロ繊維セルロースと、平均粒子径1〜1500μmの樹脂粉末とを含む、
ことを特徴とする繊維状セルロース含有物。 - 前記マイクロ繊維セルロース100質量部に対する前記樹脂粉末の配合割合が、10〜100000質量部である、
請求項1に記載の繊維状セルロース含有物。 - 前記マイクロ繊維セルロースは、平均繊維長0.02〜3.0mm、フィブリル化率1.0%以上である、
請求項1又は請求項2に記載の繊維状セルロース含有物。 - 前記マイクロ繊維セルロースが多塩基酸で変性されており、及び/又は、
前記繊維状セルロース含有物が多塩基酸を含む、
請求項1〜3のいずれか1項に記載の繊維状セルロース含有物。 - 平均繊維幅0.1μm以上のマイクロ繊維セルロースと、平均粒子径1〜1500μmの樹脂粉末とを含む繊維状セルロース含有物が乾燥されてなる、
ことを特徴とする繊維状セルロース乾燥体。 - 平均繊維幅0.1μm以上のマイクロ繊維セルロースと、平均粒子径1〜1500μmの樹脂粉末とを含む繊維状セルロース含有物の乾燥体が混練されてなる、
ことを特徴とする繊維状セルロース複合樹脂。 - 原料パルプを平均繊維幅が0.1μm以上に留まる範囲で解繊してマイクロ繊維セルロースの分散液を得、
この分散液と平均粒子径1〜1500μmの樹脂粉末とを混合する、
ことを特徴とする繊維状セルロース含有物の製造方法。 - 原料パルプを平均繊維幅が0.1μm以上に留まる範囲で解繊してマイクロ繊維セルロースの分散液を得、
この分散液と平均粒子径1〜1500μmの樹脂粉末とを混合して繊維状セルロース含有物を得、
この繊維状セルロース含有物を、含水率が95%以下となるように濃縮したうえで乾燥する、
ことを特徴とする繊維状セルロース乾燥体の製造方法。 - 原料パルプを平均繊維幅が0.1μm以上に留まる範囲で解繊してマイクロ繊維セルロースの分散液を得、
この分散液と平均粒子径1〜1500μmの樹脂粉末とを混合して繊維状セルロース含有物を得、
この繊維状セルロース含有物を乾燥して繊維状セルロース乾燥体を得、
この繊維状セルロース乾燥体を混練する、
ことを特徴とする繊維状セルロース複合樹脂の製造方法。 - 前記繊維状セルロース乾燥体と樹脂ペレットとを混練するものとし、
前記繊維状セルロース乾燥体は、前記マイクロ繊維セルロース100質量部に対して樹脂粉末が10000質量部以下の配合割合で含まれるものとし、
前記樹脂粉末100質量部に対する前記樹脂ペレットの配合割合を10〜100000質量部とする、
請求項9に記載の繊維状セルロース複合樹脂の製造方法。
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JP2013189574A (ja) * | 2012-03-14 | 2013-09-26 | Fuji Xerox Co Ltd | 樹脂組成物および樹脂成形体 |
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WO2019156047A1 (ja) * | 2018-02-06 | 2019-08-15 | 大王製紙株式会社 | 繊維状セルロース及びその製造方法、並びに樹脂組成物 |
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CN112262175B (zh) | 2023-04-04 |
JP6796111B2 (ja) | 2020-12-02 |
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