JP2021025003A - 難燃化した複合繊維およびその製造方法 - Google Patents
難燃化した複合繊維およびその製造方法 Download PDFInfo
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- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229940085991 phosphate ion Drugs 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
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- 229920002635 polyurethane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 description 1
- 235000019828 potassium polyphosphate Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 125000001501 propionyl group Chemical group O=C([*])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- 238000011069 regeneration method Methods 0.000 description 1
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- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
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- 239000001488 sodium phosphate Substances 0.000 description 1
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- JDVPQXZIJDEHAN-UHFFFAOYSA-N succinamic acid Chemical compound NC(=O)CCC(O)=O JDVPQXZIJDEHAN-UHFFFAOYSA-N 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 125000001174 sulfone group Chemical group 0.000 description 1
- LTURHSAEWJPFAA-UHFFFAOYSA-N sulfuric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OS(O)(=O)=O.NC1=NC(N)=NC(N)=N1 LTURHSAEWJPFAA-UHFFFAOYSA-N 0.000 description 1
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- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- VKFFEYLSKIYTSJ-UHFFFAOYSA-N tetraazanium;phosphonato phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])(=O)OP([O-])([O-])=O VKFFEYLSKIYTSJ-UHFFFAOYSA-N 0.000 description 1
- MVGWWCXDTHXKTR-UHFFFAOYSA-J tetralithium;phosphonato phosphate Chemical compound [Li+].[Li+].[Li+].[Li+].[O-]P([O-])(=O)OP([O-])([O-])=O MVGWWCXDTHXKTR-UHFFFAOYSA-J 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 125000001730 thiiranyl group Chemical group 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 1
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 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
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 1
- 235000019798 tripotassium phosphate Nutrition 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
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 125000000297 undecanoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Abstract
Description
[1] (a)無機粒子と繊維との複合繊維であって、繊維表面の15%以上が無機粒子によって被覆されている複合繊維と、(b)水不溶性の難燃化剤と、を含有する難燃性成形物。
[2] シート形状を有する、[1]に記載の成形物。
[3] 難燃化剤がリンおよび/または窒素系難燃化剤を含む、[1]または[2]に記載の成形物。
[4] 前記繊維がセルロース繊維である、[1]〜[3]のいずれかに記載の成形物。
[5] 前記無機粒子の少なくとも一部がカルシウム、ケイ酸、マグネシウム、バリウム、アルミニウムの金属塩、あるいはチタン、銅、亜鉛を含む金属粒子である、[1]〜[4]のいずれかに記載の成形物。
[6] [1]〜[5]のいずれかに記載の成形物の製造方法であって、複合繊維と水不溶性の難燃化剤とを含有するスラリーから成形物を得る工程を含む、上記方法。
[7] 前記複合繊維を、繊維を含有する液体中で無機粒子を合成することによって調製する、[6]に記載方法。
[8] 複合繊維と水不溶性の難燃化剤とを含有するスラリーから抄紙することによってシートを形成する、[6]または[7]に記載の方法。
本発明において「難燃」とは燃え難いこと、「難燃化」とは燃え難くすること、「難燃組成物(「難燃剤」、「難燃化剤」ともいう)」とは材料を燃え難くするための添加剤を意味する。材料およびその用途によっては法令が整備され、「難燃」に関する詳細な基準や評価方法が規格化されている。それらの中で、炎を伴った燃焼ができないことを意味する「不燃」、火が燃え広がらないことを意味する「防炎」、その他「防火」および「耐火」などの用語が使われているが、本発明では、これらの用語をすべて含めて「難燃」と定義する。
本発明は、無機粒子によってその表面が被覆された繊維を使用する。特に本発明においては、繊維表面の15%以上が無機粒子によって被覆されている複合繊維(繊維・無機複合体)を使用する。
本発明において、繊維と複合化する無機粒子は特に制限されないが、水に不溶性または難溶性の無機粒子であることが好ましい。無機粒子の合成を水系で行う場合があり、また、繊維複合体を水系で使用することもあるため、無機粒子が水に不溶性または難溶性であると好ましい。
本発明に係る複合繊維を合成する場合、キャビテーション気泡の存在下で無機粒子を析出させることができる。本発明においてキャビテーションとは、流体の流れの中で圧力差により短時間に泡の発生と消滅が起きる物理現象であり、空洞現象とも言われる。キャビテーションによって生じる気泡(キャビテーション気泡)は、流体の中で圧力がごく短時間だけ飽和蒸気圧より低くなったとき、液体中に存在する100ミクロン以下のごく微小な「気泡核」を核として生じる。
本発明においては、反応容器内に炭酸ガスを含む気体と液体を噴射することによって炭酸ガスを含むウルトラファインバブルを発生させることができる。ウルトラファインバブルの平均粒子径は1000nm以下であれば特に制限されず、好ましくは1〜800nmであり、より好ましくは10〜500nmであり、50〜300nmとしてもよい。本発明においては、高い圧力で液体を噴射することによってキャビテーション気泡を発生させる必要がないので、大きなエネルギーを消費することなく炭酸カルシウムなどの無機粒子を合成することが可能になる。
液体噴射によってウルトラファインバブルを発生させる場合、反応溶液である消石灰の水性懸濁液の固形分濃度は30重量%以下であることが好ましく、20重量%以下がより好ましい。このような濃度であると、気泡を反応系に均一に作用させやすくなるためである。また、反応溶液である消石灰の水性懸濁液は、反応効率の点から、固形分濃度が0.1重量%以上であることが好ましい。
本発明の一つの態様において、繊維を含む溶液中で無機粒子を合成することによって複合体を合成することができるが、無機粒子の合成方法は、それぞれ、公知の方法によることができる。
本発明で使用する複合繊維は、セルロース繊維と無機粒子とを複合化したものである。複合繊維を構成するセルロース繊維としては例えば、天然のセルロース繊維はもちろん、レーヨンやリヨセルなどの再生繊維(半合成繊維)や合成繊維などを制限なく使用することができる。セルロース繊維の原料としては、植物由来のパルプ繊維、セルロースナノファイバー、バクテリアセルロース、ホヤなどの動物由来セルロース、藻類などが例示され、木材パルプは、木材原料をパルプ化して製造すればよい。木材原料としては、アカマツ、クロマツ、トドマツ、エゾマツ、ベニマツ、カラマツ、モミ、ツガ、スギ、ヒノキ、カラマツ、シラベ、トウヒ、ヒバ、ダグラスファー、ヘムロック、ホワイトファー、スプルース、バルサムファー、シーダ、パイン、メルクシマツ、ラジアータパイン等の針葉樹、及びこれらの混合材、ブナ、カバ、ハンノキ、ナラ、タブ、シイ、シラカバ、ハコヤナギ、ポプラ、タモ、ドロヤナギ、ユーカリ、マングローブ、ラワン、アカシア等の広葉樹及びこれらの混合材が例示される。
本発明に係る複合繊維は、種々の形状で用いることができ、例えば、粉体、ペレット、モールド(成型体)、水性懸濁液、ペースト、シート、ボード、ブロック、糸、その他の形状にして用いることができる。また、複合繊維を主成分として他の材料と共にモールドや粒子・ペレットなどの成形体にすることもできる。乾燥して紛体にする場合の乾燥機についても特に制限はないが、例えば、気流乾燥機、バンド乾燥機、噴霧乾燥機などを好適に使用することができる。
本発明品で製造した成形物には印刷を施すことができる。この印刷方法は特に限定されるものではいが、例えば、オフセット印刷、シルクスクリーン印刷、スクリーン印刷、グラビア印刷、マイクログラビア印刷、フレキソ印刷、活版印刷、シール印刷、フォーム印刷、オンデマンド印刷、ファニッシャーロール印刷、インクジェット印刷等の公知の方式で行うことができる。この中でもインクジェト印刷は、オフセット印刷のように版下を作製する必要がなく、インクジェットプリンターの大型化が比較的容易であるため、大型シートへの印刷も可能であるため好ましい。また、フレキソ印刷は表面の凹凸が比較的大きい成形物にも好適に印刷できるため、ボードやモールド、ブロックのような形状に成形した際にも好適に用いることができる。
実験1.複合繊維の合成と評価
(サンプル1) 炭酸カルシウム粒子とセルロース繊維との複合繊維
図1に示すような反応装置を用いて、消石灰(405g、奥多摩工業製)とパルプ繊維(300g、LBKP/NBKP=8/2、CSF=377mL)とを含む水性懸濁液に対して、反応開始温度を約15℃、炭酸ガスの吹き込み量を3L/minとして反応を行い、反応液のpHが7〜8になった段階で反応を停止した。具体的には、せん断式ウルトラファインバブル発生装置(図2、エンバイロビジョン社YJ−9)に炭酸ガスを給気し、炭酸ガスを含む大量のウルトラファインバブル(平均粒子径:137nm、気泡の存在時間:60分間以上)を反応液中に発生させ、炭酸カルシウム粒子を炭酸ガス法によってセルロース繊維上に析出させ、サンプル1の複合繊維を合成した(図3)。
反応容器(マシンチェスト、容積:4m3)に2%のパルプスラリー(広葉樹晒クラフトパルプ/針葉樹晒クラフトパルプ=8/2、CSF=390mL、平均繊維長:約1.3mm、固形分25kg)と水酸化バリウム八水和物(日本化学工業、75kg)とを投入して混合後、ペリスターポンプを用いて硫酸アルミニウム(硫酸バンド、98kg)を約500g/minで滴下した。滴下終了後、そのまま30分間撹拌を継続してサンプル2を得た(図4)。
複合繊維のスラリー(固形分換算で3g)について、ろ紙を用いて吸引濾過した後、残渣をオーブンで乾燥し(105℃、2時間)、複合繊維の繊維:無機粒子の重量比を測定した。
実験1で合成した複合繊維を以下の手順によりシート化して評価した。各シートの坪量はJIS P 8124:1998、灰分はJIS P 8251:2003に基づいて測定した。
サンプル1の水性懸濁液(固形分濃度:約0.7%)101.5gと水不溶性の難燃化剤(リン・窒素系、ノンネンR165−6、丸菱油化工業製、固体)0.71gを混合し、濾紙(ADVANTEC製、標準用濾紙 No.5B、直径90mm)がセットされたブフナー漏斗に注いだ。10秒間静置後、吸引濾過によって得られた湿紙を緊張乾燥することで複合繊維シートを製造した(直径:約95mm、坪量:約200g/m2、薬剤含有率:50%)。
水不溶性の難燃化剤としてAPA−100(亜リン酸アルミニウム、太平化学工業製)を用いる以外は、上記シート1と同様にして複合繊維シートを製造した(直径:約95mm、坪量:約200g/m2、薬剤含有率:50%)。
サンプル1の水性懸濁液(約0.5%)402gと、水不溶性の難燃化剤ノンネンR165−6(リン・窒素系化合物、丸菱油化工業製)0.40gに、カチオン性歩留剤(ND300、ハイモ社製)を200ppm、アニオン性歩留剤(FA230、ハイモ社製)を200ppm添加し、500rpmにて撹拌して懸濁液を調成した。得られた懸濁液からJIS P 8222に基づいて円形手抄き器にて複合繊維シートを製造した(坪量:約120g/m2、薬剤含有率:17%)。
水不溶性の難燃化剤としてAPA−100(亜リン酸アルミニウム、太平化学工業製)を用いる以外は、上記シート3と同様にして複合繊維シートを製造した(坪量:約120g/m2、薬剤含有率:17%)。
サンプル1の水性懸濁液(濃度:約0.7%)に、アニオン性の歩留剤(FA230、ハイモ)とカチオン性の歩留剤(ND300、ハイモ)を対固形分で200ppmずつ添加して懸濁液を調製した。次いで、長網抄紙機を用いて、抄速10m/minの条件でこのスラリーからシートを製造した(坪量:約120g/m2、灰分:約60%、薬剤含有率:0%)。
難燃化剤として水溶性難燃剤(ホウ素系、BestBoron、SOUFA社製)0.40gを用いる以外は、上記シート3と同様にして複合繊維シートを製造した(坪量:約120g/m2、薬剤含有率:5%)。
サンプル2の水性懸濁液を用いた以外は、上記シート3と同様にして複合繊維シートを作製した(坪量:約120g/m2、薬剤含有率:17%)。
サンプル2の水性懸濁液を用いた以外は、上記シート6と同様にして複合繊維シートを作製した(坪量:約120g/m2、薬剤含有率:5%)。
得られたシート1〜8の燃焼性(防炎性)を、以下の手順により評価した。まず、それぞれのサンプルを70℃で3時間乾燥した後,乾燥用シリカゲルを入れたデシケータ中に2時間放置し、下記の燃焼性試験に供した。
Claims (8)
- (a)無機粒子と繊維との複合繊維であって、繊維表面の15%以上が無機粒子によって被覆されている複合繊維と、
(b)水不溶性の難燃化剤と、
を含有する難燃性成形物。 - シート形状を有する、請求項1に記載の成形物。
- 難燃化剤がリンおよび/または窒素系難燃化剤を含む、請求項1または2に記載の成形物。
- 前記繊維がセルロース繊維である、請求項1〜3のいずれかに記載の成形物。
- 前記無機粒子の少なくとも一部がカルシウム、ケイ酸、マグネシウム、バリウム、アルミニウムの金属塩、あるいはチタン、銅、亜鉛を含む金属粒子である、請求項1〜4のいずれかに記載の成形物。
- 請求項1〜5のいずれかに記載の成形物の製造方法であって、
複合繊維と水不溶性の難燃化剤とを含有するスラリーから成形物を得る工程を含む、上記方法。 - 前記複合繊維を、繊維を含有する液体中で無機粒子を合成することによって調製する、請求項6に記載方法。
- 複合繊維と水不溶性の難燃化剤とを含有するスラリーから抄紙することによってシートを形成する、請求項6または7に記載の方法。
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