JP6914758B2 - Manufacturing method of cellulose nanofiber reinforced resin - Google Patents
Manufacturing method of cellulose nanofiber reinforced resin Download PDFInfo
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- JP6914758B2 JP6914758B2 JP2017134554A JP2017134554A JP6914758B2 JP 6914758 B2 JP6914758 B2 JP 6914758B2 JP 2017134554 A JP2017134554 A JP 2017134554A JP 2017134554 A JP2017134554 A JP 2017134554A JP 6914758 B2 JP6914758 B2 JP 6914758B2
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- 239000011347 resin Substances 0.000 title claims description 42
- 229920005989 resin Polymers 0.000 title claims description 42
- 229920002678 cellulose Polymers 0.000 title claims description 28
- 239000001913 cellulose Substances 0.000 title claims description 28
- 239000002121 nanofiber Substances 0.000 title claims description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 230000002209 hydrophobic effect Effects 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 2
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002655 kraft paper Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229930182556 Polyacetal Natural products 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229920000704 biodegradable plastic Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Description
本発明は、樹脂にセルロースナノファイバーを均一に分散させたセルロースナノファイバー強化樹脂の製造方法に関するものである。 The present invention relates to a method for producing a cellulose nanofiber reinforced resin in which cellulose nanofibers are uniformly dispersed in a resin.
植物繊維をナノレベルまで微細化して得られたセルロースナノファイバーは、鉄鋼の１／５程度の軽さであり、鉄鋼の５倍以上の強度を有し、しかもガラスの１／５０の低線熱膨張係数を示す繊維である。従ってセルロースナノファイバーを樹脂に添加することで、軽量・高強度で熱による寸法変化が小さい複合材料を実現することができると期待されている。ここでセルロースナノファイバーは、樹脂との相溶性が低いことから、樹脂に均一に分散させる場合には、セルロースナノファイバーの表面を疎水化処理して樹脂との相溶性を高める必要がある。 Cellulose nanofibers obtained by refining plant fibers to the nano level are about 1/5 lighter than steel, have more than 5 times the strength of steel, and have a low coefficient of linear thermal expansion of 1/50 of glass. It is a fiber showing an expansion coefficient. Therefore, by adding cellulose nanofibers to the resin, it is expected that a composite material that is lightweight, has high strength, and has little dimensional change due to heat can be realized. Here, since the cellulose nanofibers have low compatibility with the resin, it is necessary to improve the compatibility with the resin by hydrophobizing the surface of the cellulose nanofibers in order to uniformly disperse the cellulose nanofibers in the resin.
特許文献１には、疎水化したパルプと樹脂とを混練し、同時に疎水化したパルプを解繊してセルロースナノファイバーが分散した樹脂を製造する方法が開示されている。 Patent Document 1 discloses a method of kneading a hydrophobic pulp and a resin, and at the same time defibrating the hydrophobic pulp to produce a resin in which cellulose nanofibers are dispersed.
従来はシート状のパルプをセパラブルフラスコに入れた無水酢酸に浸し、１００℃程度の温度で疎水化反応を行わせる等して疎水化パルプを製造していた。しかしながら、このような方法で疎水化パルプを製造する場合には、疎水化反応の均一性が維持できない場合があり、また疎水化反応に時間がかかる等の問題があり、セルロースナノファイバー強化樹脂の製造量を増大させることが困難であった。 Conventionally, hydrophobic pulp has been produced by immersing sheet-shaped pulp in acetic anhydride placed in a separable flask and causing a hydrophobic reaction at a temperature of about 100 ° C. However, when hydrophobized pulp is produced by such a method, the uniformity of the hydrophobizing reaction may not be maintained, and there are problems such as the hydrophobizing reaction taking a long time. It was difficult to increase the production volume.
本発明は、製造量を増大させ効率的に製造を行うことができるセルロースナノファイバー強化樹脂の製造方法を提供することを目的とする。 An object of the present invention is to provide a method for producing a cellulose nanofiber reinforced resin, which can be produced efficiently by increasing the production amount.
本発明は、以下の（１）及び（２）を提供する。
（１）下記（Ａ）〜（Ｇ）の工程を有することを特徴とするセルロースナノファイバー強化樹脂の製造方法。
工程（Ａ）：ミキサーのドラム内にパルプを投入し該パルプを解砕する工程、
工程（Ｂ）：前記ドラム内に疎水化処理を行う薬液を投入する工程、
工程（Ｃ）：前記ドラム内において前記パルプの疎水化処理を行う工程、
工程（Ｄ）：前記ドラムから疎水化パルプを抜出する工程、
工程（Ｅ）：工程（Ｄ）において抜出した前記疎水化パルプ及び樹脂を多軸押し出し機 に投入する工程、
工程（Ｆ）：前記多軸押し出し機において前記疎水化パルプ及び前記樹脂を混練する工 程、
工程（Ｇ）：前記多軸押し出し機からセルロースナノファイバー強化樹脂を排出する工 程。
（２）前記ミキサーは、レーディゲミキサーであることを特徴とする（１）記載のセルロースナノファイバー強化樹脂の製造方法。
The present invention provides the following (1) and (2).
(1) A method for producing a cellulose nanofiber reinforced resin, which comprises the following steps (A) to (G).
Step (A): A step of putting pulp into a drum of a mixer and crushing the pulp.
Step (B): A step of pouring a chemical solution to be hydrophobized into the drum.
Step (C): A step of hydrophobizing the pulp in the drum.
Step (D): A step of extracting the hydrophobic pulp from the drum,
Step (E): A step of charging the hydrophobic pulp and resin extracted in step (D) into a multi-screw extruder.
Step (F): A process of kneading the hydrophobic pulp and the resin in the multi-screw extruder.
Step (G): A process for discharging the cellulose nanofiber reinforced resin from the multi-screw extruder.
(2) The method for producing a cellulose nanofiber reinforced resin according to (1), wherein the mixer is a Ladyge mixer.
本発明によれば、製造量を増大させ効率的に製造を行うことができるセルロースナノファイバー強化樹脂の製造方法を提供することができる。 According to the present invention, it is possible to provide a method for producing a cellulose nanofiber reinforced resin, which can be produced efficiently by increasing the production amount.
本発明において、セルロースナノファイバー強化樹脂とは、セルロースナノファイバーと樹脂を含む混合物であり、セルロースナノファイバーの含有量は樹脂に対して１〜５０質量％程度である。 In the present invention, the cellulose nanofiber reinforced resin is a mixture containing cellulose nanofibers and a resin, and the content of the cellulose nanofibers is about 1 to 50% by mass with respect to the resin.
本発明の実施の形態に係るセルロースナノファイバー強化樹脂の製造方法について説明する。 A method for producing a cellulose nanofiber reinforced resin according to an embodiment of the present invention will be described.
まず、ミキサーのドラム内にパルプを投入しパルプを解砕する（工程Ａ）。ミキサーには、レーディゲミキサーを使用する。レーディゲミキサーは、横型ドラム、横型ドラムの中に設置され所定速度で回転駆動される主軸、主軸に固定された所定形状のすき状ショベル、及び高速回転するチョッパーを備えている。横型ドラム内のすき状ショベルを回転させることにより処理物を三次元流動させて混合する。またチョッパーを高速回転させることによりダマと呼ばれる塊を破砕する。またパルプは特に限定されるものではないが、繊維の強度が強い針葉樹由来の未晒クラフトパルプ（ＮＵＫＰ）を用いることが好ましい。 First, the pulp is put into the drum of the mixer and the pulp is crushed (step A). A Ladyge mixer is used as the mixer. The Ladyge mixer includes a horizontal drum, a spindle installed in the horizontal drum and driven to rotate at a predetermined speed, a plow-shaped excavator having a predetermined shape fixed to the spindle, and a chopper that rotates at a high speed. By rotating the plow-shaped excavator in the horizontal drum, the processed material is three-dimensionally flowed and mixed. Also, by rotating the chopper at high speed, a lump called lump is crushed. The pulp is not particularly limited, but it is preferable to use unbleached kraft pulp (NUKP) derived from coniferous trees having strong fiber strength.
工程Ａにおいて、レーディゲミキサーの操業条件は特に限定されるものではないが、主軸の回転数は１０〜３００ｒｐｍ、チョッパーの回転数は１２００〜３６００ｒｐｍ、ドラム内温度は１０〜８０℃、ドラム内圧力（常圧）の範囲で調整して、パルプを解砕することが好ましい。 In step A, the operating conditions of the Ladyge mixer are not particularly limited, but the rotation speed of the spindle is 10 to 300 rpm, the rotation speed of the chopper is 1200 to 3600 rpm, the temperature inside the drum is 10 to 80 ° C., and the inside of the drum. It is preferable to crush the pulp by adjusting it in the range of pressure (normal pressure).
次にミキサーのドラム内にパルプの疎水化処理を行う薬液を投入する（工程Ｂ）。パルプの疎水化処理を行う薬液には、酢酸、無水酢酸、有機酸、アミン等を用いる。 Next, a chemical solution for hydrophobizing the pulp is put into the drum of the mixer (step B). Acetic acid, acetic anhydride, organic acid, amine and the like are used as the chemical solution for hydrophobizing the pulp.
次に、ミキサーのドラム内においてパルプの疎水化処理を行う（工程Ｃ）。即ちレーディゲミキサーの横型ドラム内に、例えば未晒針葉樹クラフトパルプ（ＮＵＫＰ）及び無水酢酸等の薬液を投入し、すき状ショベルを回転させることによりパルプ及び疎水化処理を行う薬液を撹拌し、更にチョッパーによりダマと呼ばれる塊を破砕してパルプの疎水化処理をおこない、パルプ表面に存在する水酸基を疎水性の官能基で置換した疎水化パルプを製造する。 Next, the pulp is hydrophobized in the drum of the mixer (step C). That is, a chemical solution such as unbleached coniferous kraft pulp (NUKP) and anhydrous acetic acid is put into the horizontal drum of the Ladyge mixer, and the pulp and the chemical solution to be hydrophobized are stirred by rotating the plow-shaped excavator. Further, a lump called lump is crushed by a chopper to hydrophobize the pulp, and a hydrophobic pulp in which the hydroxyl group existing on the pulp surface is replaced with a hydrophobic functional group is produced.
工程Ｂ及び工程Ｃにおけるレーディゲミキサーの操業条件は、主軸の回転数は１０〜３００ｒｐｍ、チョッパーの回転数は１２００〜３６００ｒｐｍ、ドラム内温度は５０〜１２０℃、ドラム内圧力は常圧の範囲で調整して、疎水化反応を行い、疎水化パルプを製造することが好ましい。 The operating conditions of the Radige mixer in steps B and C are that the rotation speed of the spindle is 10 to 300 rpm, the rotation speed of the chopper is 1200 to 3600 rpm, the temperature inside the drum is 50 to 120 ° C, and the pressure inside the drum is in the range of normal pressure. It is preferable to carry out a hydrophobization reaction to produce hydrophobized pulp.
次に、ミキサーのドラムから未反応の無水酢酸等の薬液を留去する。（工程Ｄ）。即ち疎水化処理により製造された疎水化パルプを減圧し、薬液を蒸発させレーディゲミキサーの横型ドラムから抜出する。 Next, an unreacted chemical solution such as acetic anhydride is distilled off from the drum of the mixer. (Step D). That is, the hydrophobized pulp produced by the hydrophobizing treatment is depressurized, the chemical solution is evaporated, and the pulp is extracted from the horizontal drum of the Ladige mixer.
工程Ｄにおける操業条件は、主軸の回転数１０〜３００ｒｐｍ、チョッパーの回転数は１２００〜３６００ｒｐｍ、ドラム内温度は６０〜１３０℃、ドラム内圧力は０〜５０Ｔｏｒｒの範囲で調整して、未反応の無水酢酸等の薬液を留去する。未反応薬液留去後、疎水化パルプを抜出する。 The operating conditions in step D are that the rotation speed of the spindle is 10 to 300 rpm, the rotation speed of the chopper is 1200 to 3600 rpm, the temperature inside the drum is 60 to 130 ° C., and the pressure inside the drum is adjusted in the range of 0 to 50 Torr, and there is no reaction. Distillate a chemical solution such as acetic anhydride. After distilling off the unreacted chemical solution, the hydrophobic pulp is extracted.
次に、レーディゲミキサーの横型ドラムから抜出した疎水化パルプ及び樹脂を多軸押し出し機に投入する（工程Ｅ）。ここで樹脂への疎水化パルプの配合比率は、１〜５０％が好ましい。多軸押し出し機としては、４軸押し出し機を用いる。４軸押し出し機は、バレル内に４本のスクリューを備え、４本のスクリューを同方向または異方向に回転させながら樹脂を混練し定量で押し出す。 Next, the hydrophobic pulp and the resin extracted from the horizontal drum of the Ladyge mixer are put into the multi-screw extruder (step E). Here, the blending ratio of the hydrophobic pulp to the resin is preferably 1 to 50%. As the multi-axis extruder, a 4-axis extruder is used. The 4-axis extruder is provided with four screws in the barrel, and the resin is kneaded and extruded in a fixed amount while rotating the four screws in the same direction or different directions.
樹脂としては、ポリアミド系、ポリオレフィン系、フッ化ポリオレフィン系、ポリアセタール系、ポリイミド系、アクリル樹脂系、生分解性プラスチック系、エポシキ樹脂系等の樹脂を用いる。 As the resin, resins such as polyamide-based, polyolefin-based, fluoropolyolefin-based, polyacetal-based, polyimide-based, acrylic resin-based, biodegradable plastic-based, and Eposiki resin-based resins are used.
次に、多軸押し出し機において疎水化パルプ及び樹脂を混練する（工程Ｆ）。即ち４軸押し出し機の４軸のスクリューの回転により疎水化パルプと樹脂とを混練し、同時に疎水化したパルプを解繊してセルロースナノファイバーを樹脂に均一に分散させる。 Next, the hydrophobic pulp and the resin are kneaded in a multi-screw extruder (step F). That is, the hydrophobic pulp and the resin are kneaded by the rotation of the 4-axis screw of the 4-axis extruder, and at the same time, the hydrophobic pulp is defibrated to uniformly disperse the cellulose nanofibers in the resin.
次に、多軸押し出し機からセルロースナノファイバー強化樹脂を排出する（工程Ｇ）。 Next, the cellulose nanofiber reinforced resin is discharged from the multi-axis extruder (step G).
即ち上述の工程Ａ〜工程Ｇにより、セルロースナノファイバーが均一に分散したセルロースナノファイバー強化樹脂の製造することができる。 That is, by the above-mentioned steps A to G, a cellulose nanofiber reinforced resin in which cellulose nanofibers are uniformly dispersed can be produced.
本実施の形態に係るセルロースナノファイバー強化樹脂の製造方法によれば、パルプの疎水化処理をレーディゲミキサーを用いて行っているため、チョッパーによりダマを破砕することができ疎水化反応の反応性や反応の均一性を高めることができる。従って疎水化パルプの歩留まりを増加させることができる。また疎水化反応の反応時間を短縮することができる。更に製造設備のスケールアップも容易に行うことができる。 According to the method for producing a cellulose nanofiber reinforced resin according to the present embodiment, since the pulp is hydrophobized using a Ladyge mixer, the lumps can be crushed by a chopper and the reactivity of the hydrophobization reaction. It is possible to improve the uniformity of sex and reaction. Therefore, the yield of hydrophobized pulp can be increased. Moreover, the reaction time of the hydrophobization reaction can be shortened. Further, the scale-up of the manufacturing equipment can be easily performed.
なお上述の実施の形態においては、ミキサーとしてレーディゲミキサーを用いているが、竪型のヘンシェルミキサーを用いてもよい。竪型ヘンシェルミキサーは、竪型の混合槽、混合槽の下部に設置された上羽根及び下羽根を備えている。混合槽内で上羽根及び下羽根を回転させることにより、混合槽内の処理物は下羽根の回転により旋回しながら上下方向に流動し、対流した処理物に上羽根によりせん断力を付与することにより処理物を短時間で混合する。 In the above-described embodiment, the Ladyge mixer is used as the mixer, but a vertical Henschel mixer may be used. The vertical Henschel mixer includes a vertical mixing tank and upper and lower blades installed at the bottom of the mixing tank. By rotating the upper and lower blades in the mixing tank, the processed material in the mixing tank flows in the vertical direction while swirling due to the rotation of the lower blade, and the convected processed material is given a shearing force by the upper blade. The processed material is mixed in a short time.
また上述の実施の形態においては多軸押し出し機として４軸押し出し機を用いているが、２軸押し出し機、または８軸押し出し機等を用いてもよい。 Further, in the above-described embodiment, the 4-axis pusher is used as the multi-axis pusher, but a 2-axis pusher, an 8-axis pusher, or the like may be used.
（レーディゲミキサーの仕様）
真空乾燥タイプの横型ドラム（１２００Ｌ）を備えたレーディゲミキサー。
（４軸押し出し機の仕様）
同方向完全噛合型４軸混練押出機（株式会社テクノベル製）。
（操業条件）
ＮＵＫＰの解砕は、ショベルが設置された主軸の回転数（１００ｒｐｍ）、チョッパーの回転数（１２００〜３６００ｒｐｍ）、ドラム内温度（５０℃）、ドラム内圧力（常圧）で行う。
(Specifications of Lai Gemixer)
A Ladyge mixer equipped with a vacuum-drying horizontal drum (1200L).
(Specifications of 4-axis extruder)
Same-direction perfect mesh 4-screw kneading extruder (manufactured by Technobel Co., Ltd.).
(Operating conditions)
NUKP is crushed at the rotation speed (100 rpm) of the spindle on which the excavator is installed, the rotation speed of the chopper (1200 to 3600 rpm), the temperature inside the drum (50 ° C.), and the pressure inside the drum (normal pressure).
その後、ドラム内へ無水酢酸等の薬液を投入し、ショベルが設置された主軸の回転数（１００ｒｐｍ）、チョッパーの回転数（１２００〜３６００ｒｐｍ）、ドラム内温度（８０℃）、ドラム内圧力（常圧）で疎水化反応を行い疎水化パルプを製造する。 After that, a chemical solution such as acetic anhydride is poured into the drum, and the rotation speed of the spindle on which the excavator is installed (100 rpm), the rotation speed of the chopper (1200 to 3600 rpm), the temperature inside the drum (80 ° C.), and the pressure inside the drum (normal). The hydrophobization reaction is carried out by pressure) to produce hydrophobized pulp.
反応終了後、未反応の無水酢酸等の薬液をショベルが設置された主軸の回転数（１００ｒｐｍ）、チョッパーの回転数（１２００〜３６００ｒｐｍ）、ドラム内温度（１０５℃）、ドラム内圧力（５０Ｔｏｒｒ）で留去する。未反応薬液留去後、疎水化パルプを抜出する。 After the reaction is completed, unreacted chemical solution such as acetic anhydride is applied to the spindle rotation speed (100 rpm) on which the excavator is installed, the chopper rotation speed (1200 to 3600 rpm), the drum temperature (105 ° C.), and the drum pressure (50 Torr). To stay away. After distilling off the unreacted chemical solution, the hydrophobic pulp is extracted.
次に４軸押し出し機に疎水化パルプ及び樹脂を投入する。樹脂への疎水化パルプの配合比率は、３０％とする。４軸押し出し機により疎水化パルプ及び樹脂を混練し、同時に疎水化パルプを解繊して樹脂にセルロースナノファイバーを均一に分散させる。４軸押し出し機からセルロースナノファイバーが均一に分散したセルロースナノファイバー強化樹脂を排出する。 Next, the hydrophobic pulp and the resin are put into the 4-screw extruder. The mixing ratio of the hydrophobic pulp to the resin is 30%. The hydrophobic pulp and the resin are kneaded by a 4-axis extruder, and at the same time, the hydrophobic pulp is defibrated to uniformly disperse the cellulose nanofibers in the resin. The cellulose nanofiber reinforced resin in which the cellulose nanofibers are uniformly dispersed is discharged from the 4-axis extruder.
Claims (1)
工程（Ａ）：チョッパーを備えるレーディゲミキサーのドラム内にパルプを投入し該パルプを解砕する工程、
工程（Ｂ）：前記ドラム内に疎水化処理を行う薬液を投入する工程、
工程（Ｃ）：前記ドラム内において、前記チョッパーにより前記パルプの塊を破砕しながら前記パルプの疎水化処理を行う工程であって、前記レーディゲミキサーの操業条件は、主軸の回転数が１０〜３００ｒｐｍ、前記チョッパーの回転数が１２００〜３６００ｒｐｍ、前記ドラム内の温度が５０〜１２０℃、前記ドラム内の圧力が常圧である工程、
工程（Ｄ）：前記ドラムから疎水化パルプを抜出する工程、
工程（Ｅ）：工程（Ｄ）において抜出した前記疎水化パルプ及び樹脂を多軸押し出し機 に投入する工程、
工程（Ｆ）：前記多軸押し出し機において前記疎水化パルプ及び前記樹脂を混練する工 程、
工程（Ｇ）：前記多軸押し出し機からセルロースナノファイバー強化樹脂を排出する工 程。 A method for producing a cellulose nanofiber reinforced resin, which comprises the following steps (A) to (G).
Step (A): A step of putting pulp into a drum of a Ladyge mixer equipped with a chopper and crushing the pulp.
Step (B): A step of pouring a chemical solution to be hydrophobized into the drum.
Step (C): A step of hydrophobizing the pulp while crushing the pulp mass by the chopper in the drum, and the operating condition of the Ladyge mixer is that the number of rotations of the spindle is 10. ~ 300 rpm, the rotation speed of the chopper is 1200 to 3600 rpm, the temperature in the drum is 50 to 120 ° C., and the pressure in the drum is normal pressure .
Step (D): A step of extracting the hydrophobic pulp from the drum,
Step (E): A step of charging the hydrophobic pulp and resin extracted in step (D) into a multi-screw extruder.
Step (F): A process of kneading the hydrophobic pulp and the resin in the multi-screw extruder.
Step (G): A process for discharging the cellulose nanofiber reinforced resin from the multi-screw extruder.
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