JP6744241B2 - 炭酸マグネシウムと繊維の複合繊維の溶解抑制 - Google Patents
炭酸マグネシウムと繊維の複合繊維の溶解抑制 Download PDFInfo
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- JP6744241B2 JP6744241B2 JP2017040771A JP2017040771A JP6744241B2 JP 6744241 B2 JP6744241 B2 JP 6744241B2 JP 2017040771 A JP2017040771 A JP 2017040771A JP 2017040771 A JP2017040771 A JP 2017040771A JP 6744241 B2 JP6744241 B2 JP 6744241B2
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- Prior art keywords
- magnesium carbonate
- acid
- fiber
- fibers
- paper
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- 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.)
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- 229910000021 magnesium carbonate Inorganic materials 0.000 title claims description 175
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 title claims description 174
- 239000002131 composite material Substances 0.000 title claims description 90
- 238000004090 dissolution Methods 0.000 title description 8
- 230000005764 inhibitory process Effects 0.000 title 1
- 238000000034 method Methods 0.000 claims description 65
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- 239000002245 particle Substances 0.000 claims description 25
- 239000002253 acid Substances 0.000 claims description 21
- 239000010954 inorganic particle Substances 0.000 claims description 18
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 15
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 27
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 25
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- 230000032683 aging Effects 0.000 description 9
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- 239000007900 aqueous suspension Substances 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
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- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 235000014786 phosphorus Nutrition 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 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
- 239000002243 precursor Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- AXLMPTNTPOWPLT-UHFFFAOYSA-N prop-2-enyl 3-oxobutanoate Chemical compound CC(=O)CC(=O)OCC=C AXLMPTNTPOWPLT-UHFFFAOYSA-N 0.000 description 1
- 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
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 235000017985 rocky mountain lodgepole pine Nutrition 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 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
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 229910001575 sodium mineral Inorganic materials 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 235000019830 sodium polyphosphate Nutrition 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000011122 softwood Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000003696 stearoyl 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])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
- 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
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229960002317 succinimide Drugs 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
- 239000012756 surface treatment agent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000003826 tablet Substances 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
- 125000002053 thietanyl group Chemical group 0.000 description 1
- 125000001730 thiiranyl group Chemical group 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 210000001519 tissue Anatomy 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
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 1
- 235000019798 tripotassium phosphate Nutrition 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 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
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 125000003774 valeryl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000002982 water resistant material Substances 0.000 description 1
- 239000002349 well water Substances 0.000 description 1
- 235000020681 well water Nutrition 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Description
MgCO3 + H2O → Mg2+ + CO2 +2OH−
複合繊維から炭酸マグネシウムが溶出することによって、炭酸マグネシウムに起因する特性が複合繊維から失われることになり、また、スラリーのpHが高くなると、アルカリ性の排水を処理するための排水処理の負荷も高まる。
(1) 炭酸マグネシウム粒子と繊維との複合繊維を改質する方法であって、繊維と複合化した炭酸マグネシウムの表面に炭酸マグネシウムよりも水への溶解度が低い無機粒子を析出させるか、多価カルボン酸、ポリリン酸またはキレート剤を吸着させる工程を含む、上記方法。
(2) 析出させる無機粒子が、水酸化アルミニウムおよび/または硫酸バリウムである、(1)に記載の方法。
(3) 多価カルボン酸がポリアクリル酸および/またはポリアクリル酸ナトリウムを含む、(1)に記載の方法。
(4) 改質された複合繊維を水中に分散して濃度が1重量%のスラリーを調製した場合、分散開始から120秒後のスラリーのpHが9.5未満である、(1)〜(3)のいずれかに記載の方法。
(5) 前記繊維がセルロース繊維である、(1)〜(4)のいずれかに記載の方法。
(6) 炭酸マグネシウムの一次粒子径が10nm〜3μmである、(1)〜(5)のいずれかに記載の方法。
(7) 炭酸マグネシウムが、塩基性炭酸マグネシウムである、(1)〜(6)のいずれかに記載の方法。
(8) 炭酸マグネシウムと繊維の重量比が10:90〜90:10である、(1)〜(7)のいずれかに記載の方法。
(9) 炭酸マグネシウム粒子と繊維との複合繊維であって、繊維と複合化した炭酸マグネシウムの表面に炭酸マグネシウムよりも水への溶解度が低い無機粒子が析出している、上記複合繊維。
(10) 炭酸マグネシウム粒子と繊維との複合繊維であって、繊維と複合化した炭酸マグネシウムの表面に多価カルボン酸、ポリリン酸またはキレート剤が吸着している、上記複合繊維。
本発明の好ましい態様において、複合繊維を水に分散して1重量%のスラリーとした場合、分散から120秒後のスラリーのpHが9.5未満であり、より好ましくは9.4以下であり、さらに好ましくは9.2以下であり、よりさらに好ましくは9.0以下とすることができる。
(水酸化マグネシウム)
MgCl2+2Na(OH)2→Mg(OH)2+2NaCl
(炭酸カルシウム)
CaCl2+Na2CO3→CaCO3+2NaCl2
(炭酸バリウム)
BaCl2+Na2CO3→BaCO3+2NaCl2
(炭酸亜鉛)
ZnSO4+Na2CO3→ZnCO3+Na2SO4
(硝酸銀)
Ag+2HNO3→AgNO3+NO2+H2O
(炭酸銀)
NaCO3+AgNO3→AgCO3+NaNO3
(炭酸鉄)
FeSO4+Na2CO3→FeCO3+Na2SO4
(炭酸銅)
CuSO4+Na2CO3→CuCO3+Na2SO4
(第一リン酸カルシウム、リン酸二水素カルシウム)
CaCO3+2H3PO4→Ca(H2PO4)2+H2O+CO2
(第二リン酸カルシウム、リン酸水素カルシウム)
CaCO3+H3PO4→CaHPO4+H2O+CO2
(第三リン酸カルシウム、リン酸三カルシウム)
CaCO3+H3PO4→Ca3(PO4)2+3H2O+3CO2
(リン酸水素バリウム)
BaCO3+H3PO4→BaHPO4+H2O+CO2
(リン酸二水素マグネシウム)
MgCO3+2H3PO4→Mg(H2PO4)2+H2O+CO2
(リン酸水素マグネシウム)
MgCO3+H3PO4→MgHPO4+H2O+CO2
(リン酸三マグネシウム)
MgCO3+H3PO4→Mg3(PO4)2+3H2O+3CO2
(シュウ酸カルシウム)
H2C2O4+Ca(OH)2→CaC2O4+2H2O
(シュウ酸銀)
H2C2O4+2AgOH→Ag2C2O4+2H2O
(シュウ酸鉄二水和物)
H2C2O4+Fe(OH)2→Fe(C2O4)・2H2O
(臭化銀)
2KBr+AgCl2→AgBr+2KCl
(酸化銀)
AgCl2+2NaOH→AgO+2NaCl+H2O
(過マンガン酸バリウム)
2KMnO4+BaCl2→Ba(MnO4)2+2KCl
(塩化銀)
AgO+2HCl→AgCl2+H2O
(シリカ)
Na2SiO3+H2SO4→SiO2+Na2SO4+H2O
また別の態様において、繊維と複合化した炭酸マグネシウムの表面に、多価カルボン酸、ポリリン酸、キレート剤などをイオン結合で吸着させることによって、炭酸マグネシウムの水への溶解を抑制する。炭酸マグネシウムとイオン結合させる物質としては、例えば、多価カルボン酸、ポリリン酸、各種キレート剤などが挙げられ、複数の物質を併用してもよい。
本発明は、炭酸マグネシウムと繊維との複合繊維に関する。本発明に係る複合繊維を構成する炭酸マグネシウム微粒子の平均粒子径は、例えば50μm未満であるが、平均粒子径が30μm以下の炭酸マグネシウムとすることもできる。また、好ましい態様において、炭酸マグネシウム微粒子の平均一次粒子径を10nm〜3μm程度とすることや、10nm〜1μmとすることも可能である。
本発明においては、炭酸マグネシウム微粒子と繊維とを複合化する。複合繊維を構成する繊維は特に制限されないが、例えば、セルロースなどの天然繊維はもちろん、石油などの原料から人工的に合成される合成繊維、さらには、レーヨンやリヨセルなどの再生繊維(半合成繊維)、さらには無機繊維などを制限なく使用することができる。天然繊維としては上記の他にウールや絹糸やコラーゲン繊維等の蛋白系繊維、キチン・キトサン繊維やアルギン酸繊維等の複合糖鎖系繊維等が挙げられる。セルロース系の原料としては、パルプ繊維(木材パルプや非木材パルプ)、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。
本発明においては、繊維を含む溶液中で炭酸マグネシウム微粒子を合成するが、炭酸マグネシウムの合成方法は、公知の方法によることができる。例えば、水酸化マグネシウムと炭酸ガスから重炭酸マグネシウムを合成し、重炭酸マグネシウムから正炭酸マグネシウムを経て塩基性炭酸マグネシウムを合成することができる。炭酸マグネシウムは合成方法によって重炭酸マグネシウム、正炭酸マグネシウム、塩基性炭酸マグネシウムなどを得ることができるが、本発明の複合繊維に係る炭酸マグネシウムは、塩基性炭酸マグネシムにすることが特に好ましい。なぜならば、重炭酸マグネシウムは安定性が比較的低く、柱状(針状)結晶である正炭酸マグネシウムは繊維へ定着しにくい場合があるためである。一方、繊維の存在下で塩基性炭酸マグネシウムにまで化学反応させることで、繊維表面をうろこ状などに被覆した炭酸マグネシウムと繊維の複合繊維を得ることができる。
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炭酸マグネシウム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。
また、容器内の圧力と噴射液の圧力との比は0.001〜0.5の範囲が好ましい。
本発明によって得られた複合繊維は、種々の形状で用いることができ、例えば、粉体、パルプ、ペレット、モールド、水性懸濁液、微小球形粒、ペースト、シート、糸、発泡体、または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、糸、発泡体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。
以下に示す手順により、炭酸マグネシウムとパルプ繊維の複合繊維を合成した。水酸化マグネシウム700g(宇部マテリアルズ、UD653)とクラフトパルプ700g(LBKP/NBKP=8/2、カナダ標準フリーネス:370ml、平均繊維長:0.9mm)を水中に添加して水性懸濁液を準備した。
(サンプル1、図3)
2AlCl3+3Mg2++6OH−→2Al(OH)3+3Mg2++6Cl-
塩化アルミニウム六水和物(和光純薬、0.9g、塩化アルミニウム換算で0.5g)を3%水溶液に調整した。実験1で得られた複合繊維のスラリー(濃度3.2%、固形分10g、pH:8.6)を室温下でスリーワンモーターにて700rpmで撹拌する中に、塩化アルミニウム水溶液をペリスターポンプにて2mL/minで滴下した(滴下終了時のpH:7.4)。全量の滴下が終了後、室温にて30分間撹拌を継続して熟成を行った。
用いる塩化アルミニウム六水和物の量を2.4g(塩化アルミニウム換算で1.3g)とした他は、サンプル1と同様にして実験を行った(滴下終了時のpH:7.2)。
塩化アルミニウム六水和物(和光純薬、9g、塩化アルミニウム換算で5g)の5%水溶液、および、水酸化ナトリウム(和光純薬)の5%水溶液を調製した。実験1で得られた複合繊維のスラリー(濃度3.2%、固形分10g)を室温下でスリーワンモーターにて700rpmで撹拌する中に、上記5%塩化アルミニウム水溶液をペリスターポンプにて2mL/minで滴下した。反応液のpHをモニターしながら、滴下中にpHが7を下回りそうになった際に、水酸化ナトリウム水溶液を1mLずつピペッターで添加した(添加した水酸化ナトリウムの固形分総量:1.8g、滴下終了時のpH:6.8)。塩化アルミニウム水溶液の全量の滴下が終了後、30分間撹拌して熟成し、炭酸マグネシウムの結晶表面に水酸化アルミニウムが析出したサンプルを製造した。
Al2(SO4)3+3Mg2++6OH−→2Al(OH)3+3Mg2++3SO4 2-
塩化アルミニウム水溶液の代わりに硫酸アルミニウム溶液(工業用硫酸バンド、10倍希釈品16.7g、アルミナ換算で0.13g)を用いた他は、サンプル1と同様にして実験を行った(滴下終了時のpH:7.7)。
用いる硫酸アルミニウム溶液を5倍希釈品とし、液の総重量を29.2g(添加した硫酸アルミニウム総量はアルミナ換算で0.47g)した他は、サンプル4と同様にして実験を行った(滴下終了時のpH:7.0)。
塩化アルミニウム六水和物の代わりに硫酸アルミニウム溶液(硫酸バンドの3倍希釈品、188g、アルミナ換算で5g)を用いた他は、サンプル3と同様にして炭酸マグネシウムの結晶表面に水酸化アルミニウムを析出させた。なお、この実験で添加した水酸化ナトリウムの固形分総量は8.1gであった(滴下終了時のpH:6.8)。
Al2(OH)3Cl3+3Mg2++3OH−→2Al(OH)3+3Mg2++3Cl-
塩化アルミニウム水溶液の代わりにポリ塩化アルミニウム溶液(PAC溶液、浅田化学100B、3倍希釈品、21.3g、アルミナ換算≧0.2g)を用いた他は、サンプル1と同様にして実験を行った(滴下終了時のpH:7.4)。
用いるポリ塩化アルミニウム溶液の重量を72.5g(アルミナ換算≧0.2g)とした他は、サンプル7と同様にして実験を行った(滴下終了時のpH:7.1)。
塩化アルミニウム六水和物の代わりにポリ塩化アルミニウム溶液(PAC、浅田化学100B、3倍希釈品、158g、アルミナ換算≧5g)を用いた他は、サンプル3と同様にして炭酸マグネシウムの結晶表面に水酸化アルミニウムを析出させた。なお、この実験で添加した水酸化ナトリウムの固形分総量は7.2gであった(滴下終了時のpH:6.9)。
3Ba(OH)2+Al2(SO4)3→3BaSO4+2Al(OH)3
実験1で得られた複合繊維のスラリー(サンプルA、濃度3.2%、固形分10g)に水酸化バリウム八水和物(和光純薬、0.7g、水酸化バリウム換算0.5g)を添加した。このスラリーを室温下でスリーワンモーターにて700rpmで撹拌する中に、硫酸アルミニウム溶液(硫酸バンドの5倍希釈品、11.6g、アルミナ換算で0.19g)をペリスターポンプにて2mL/minで滴下した(滴下終了時のpH:7.9)。全量滴下終了後、30分間撹拌を継続して熟成を行い、サンプル10を得た。
用いる水酸化バリウム八水和物の量を2.2g(水酸化バリウム換算1.5g)とし、硫酸バンドの総添加量を61.6g(アルミナ換算で1.0g)とした以外は、サンプル10と同様にして複合繊維を改質した(滴下終了時のpH:7.9)。
(サンプル12)
実験1で得られた複合繊維のスラリー(濃度0.5%、固形分0.5g)にポリアクリル酸(和光純薬、分子量5000、0.05g)を添加した(添加後のpH:7.4)。このスラリーを室温下でスリーワンモーターにて700rpmで30秒間撹拌し、サンプル12を得た。
TEMPO酸化CNF(濃度1%、固形分0.02g、製造法は以下のとおり)を用いた以外は、サンプル12と同様にしてサンプル13を得た(添加後のpH:8.3)。
<TEMPO酸化CNFの製造> 粉末セルロース(日本製紙ケミカル製、粒径24μm)15g(絶乾)を、TEMPO(Sigma Aldrich社)78mg(0.5mmol)と臭化ナトリウム755mg(7mmol)を溶解した水溶液500mlに加え、粉末セルロースが均一に分散するまで攪拌した。反応系に次亜塩素酸ナトリウム水溶液(有効塩素5%)50mlを添加した後、0.5N塩酸水溶液でpHを10.3に調整し、酸化反応を開始した。反応中は系内のpHは低下するが、0.5N水酸化ナトリウム水溶液を逐次添加し、pH10に調整した。2時間反応した後、遠心操作(6000rpm、30分、20℃)で酸化した粉末セルロースを分離し、十分に水洗することで酸化処理した粉末セルロースを得た。酸化処理した粉末セルロースの2%(w/v)スラリーをミキサーにより12,000rpm、15分処理し、さらに粉末セルローススラリーを超高圧ホモジナイザーにより140MPaの圧力で5回処理したところ、透明なゲル状分散液としてセルロースナノファイバー(CNF)が得られた。
<サンプル12および13のキレート状態の確認> 上記のようにして調整したサンプル12および13をそれぞれ100mLずつ取り、ブフナーを用いてマットとろ液に分離した(使用したろ紙:アドバンテック製、No.2)。得られたマットは、100mLの水道水に全量投入し、スリーワンモーターで600rpmの速度で1分間撹拌し、完全に離解した。離解後のマットスラリーと、ブフナーろ過で得られたろ液を、自動滴定装置(Mutek社製、PCD−03)を用い、ポリジアリルジメチルアンモニウムクロライド(DADMAC)でカチオン要求量を測定した。測定したカチオン要求量(アニオン性)から、下式に基づいて、各添加物の炭酸マグネシウム複合体への定着率を評価したところ、サンプル12の定着率は約20%、サンプル13の定着率は約92%だった。なお、ポリアクリル酸やCNF、原料の炭酸マグネシウム複合体については、サンプル12や13を調整する際に用いた濃度の水溶液のカチオン要求量を測定した。
定着率=[(添加物のカチオン要求量+炭酸マグネシウム複合体のカチオン要求量)−添加物を添加後の炭酸マグネシウム複合体マットのカチオン要求量]÷添加物のカチオン要求×100
(カチオン要求量)
・炭酸マグネシウム複合体:24(調製時スラリー)、26(マットスラリー)
・ポリアクリル酸:1029(調製時スラリー)
・CNF:290(調製時スラリー)
・炭酸マグネシウム複合体+ポリアクリル酸:845(マットスラリー)、10(ろ液)
・炭酸マグネシウム複合体+CNF:47(マットスラリー)、25(ろ液)
(サンプル14)塩酸(比較例)
塩化アルミニウム六水和物の代わりに塩酸水溶液(和光純薬、1M、22.0g、固形分0.8g)を用いた他は、サンプル1と同様にしてサンプル14を得た(添加後のpH:7.6)。
実験1および実験2で得られたそれぞれの複合繊維スラリーについて、ろ紙を用いて吸引濾過し、残渣をシートプレス機にて1MPaの圧力で2分間プレスして、直径約9cmの円形のウェットマットを作製した。
また、水への分散しやすさ(離解性)については、下記の基準により3段階で評価した。
・3点:未離解片が1〜2個以下しか認められない
・2点:未離解片が3〜6個認められる
・1点:未離解片が7個以上認められる、もしくは7mm以上の未離解片がある
MgCO3 + H2O → Mg2+ + CO2 +2OH−
それに対し、炭酸マグネシウムの表面に溶解しにくい水酸化アルミニウムや硫酸バリウムを析出させたサンプル1〜11は、水中に分散させた場合、離解後のpHの上昇が抑制されていた。また、サンプル12〜13も、離解したスラリーのpHが低く、炭酸マグネシウムとパルプの複合繊維にポリカルボン酸を添加することによって、炭酸マグネシウムの水への溶解が抑制されたものと考えられた。
実験4:燃焼試験
一般に炭酸マグネシウムは難燃材として用いられることから、実験2のサンプルをマット状にしてから、その難燃性能を確認した。
・サンプル3のマット:坪量320g/m2(灰分:約40%、図8左)
・サンプル6のマット:坪量520g/m2(灰分:約54%、図8中央)
・サンプル9のマット:坪量390g/m2(灰分:約56%、図8右)
次いで、手持ちのガスバーナーを用いて燃焼試験を行った。具体的には、ガスバーナーの先端からマットまでの間を10cm離してガスバーナーを着火し、着火10秒後におけるマットの燃焼状態を目視で評価した。
(複合繊維の改質)
実験1と同様にして合成した炭酸マグネシウム複合体をマシンチェスト(4m2)中で撹拌した(濃度3.5%、945L)。そこに工業用硫酸アルミニウム(硫酸バンド)5.3kgを、ペリスターポンプにて180g/minの早さで滴下することで、水酸化アルミニウムで表面修飾した炭酸マグネシウム複合体を得た(サンプル5−1)。
実験1の複合体と上記サンプルについて、濃度1%に希釈後、それぞれに対してND300(ハイモ社製)とFA230(ハイモ社製)を100ppmずつ添加して紙料を調製した。調整後のスラリーを、それぞれ長網抄紙機(抄速10m/min)を用いてシート化した。その際の白水(抄紙ワイヤーにてろ別されて出るろ液)のpHを測定したところ、未処理の複合体ではpHが9.1だったのに対し、サンプル5−1ではpHが8.4、サンプル5−2ではpHが8.3であった。
Claims (10)
- 炭酸マグネシウム粒子と繊維との複合繊維を改質する方法であって、
繊維と複合化した炭酸マグネシウムの表面に炭酸マグネシウムよりも水への溶解度が低い無機粒子を析出させるか、多価カルボン酸、ポリリン酸またはキレート剤を吸着させる工程を含む、上記方法。 - 析出させる無機粒子が、水酸化アルミニウムおよび/または硫酸バリウムである、請求項1に記載の方法。
- 多価カルボン酸がポリアクリル酸および/またはポリアクリル酸ナトリウムを含む、請求項1に記載の方法。
- 改質された複合繊維を水中に分散して濃度が1重量%のスラリーを調製した場合、分散開始から120秒後のスラリーのpHが9.5未満である、請求項1〜3のいずれかに記載の方法。
- 前記繊維がセルロース繊維である、請求項1〜4のいずれかに記載の方法。
- 炭酸マグネシウムの平均一次粒子径が10nm〜3μmである、請求項1〜5のいずれかに記載の方法。
- 炭酸マグネシウムが、塩基性炭酸マグネシウムである、請求項1〜6のいずれかに記載の方法。
- 炭酸マグネシウムと繊維の重量比が10:90〜90:10である、請求項1〜7のいずれかに記載の方法。
- 炭酸マグネシウム粒子と繊維との複合繊維であって、
繊維と複合化した炭酸マグネシウムの表面に炭酸マグネシウムよりも水への溶解度が低い無機粒子が析出している、上記複合繊維。 - 炭酸マグネシウム粒子と繊維との複合繊維であって、
繊維と複合化した炭酸マグネシウムの表面に多価カルボン酸、ポリリン酸またはキレート剤が吸着している、上記複合繊維。
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