JP2014008497A - イオン交換能を有する粒状体の製造方法 - Google Patents
イオン交換能を有する粒状体の製造方法 Download PDFInfo
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- JP2014008497A JP2014008497A JP2012149162A JP2012149162A JP2014008497A JP 2014008497 A JP2014008497 A JP 2014008497A JP 2012149162 A JP2012149162 A JP 2012149162A JP 2012149162 A JP2012149162 A JP 2012149162A JP 2014008497 A JP2014008497 A JP 2014008497A
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- filler
- cation exchange
- aqueous solution
- alginate
- granular material
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 title abstract description 4
- 239000000945 filler Substances 0.000 claims abstract description 74
- 235000010443 alginic acid Nutrition 0.000 claims abstract description 37
- 229920000615 alginic acid Polymers 0.000 claims abstract description 37
- 239000007864 aqueous solution Substances 0.000 claims abstract description 36
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims abstract description 33
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
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- 238000005349 anion exchange Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 14
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 7
- 229910021536 Zeolite Inorganic materials 0.000 claims description 7
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 7
- 235000010413 sodium alginate Nutrition 0.000 claims description 7
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- 239000003957 anion exchange resin Substances 0.000 description 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 4
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 229910052792 caesium Inorganic materials 0.000 description 3
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
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- 239000012670 alkaline solution Substances 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
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- 238000010998 test method Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 241001311547 Patina Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- CANRESZKMUPMAE-UHFFFAOYSA-L Zinc lactate Chemical compound [Zn+2].CC(O)C([O-])=O.CC(O)C([O-])=O CANRESZKMUPMAE-UHFFFAOYSA-L 0.000 description 1
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 229910001583 allophane Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229940010048 aluminum sulfate Drugs 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 235000010407 ammonium alginate Nutrition 0.000 description 1
- 239000000728 ammonium alginate Substances 0.000 description 1
- KPGABFJTMYCRHJ-YZOKENDUSA-N ammonium alginate Chemical compound [NH4+].[NH4+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O KPGABFJTMYCRHJ-YZOKENDUSA-N 0.000 description 1
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- HLKMEIITONDPGG-UHFFFAOYSA-L barium(2+);2-hydroxypropanoate Chemical compound [Ba+2].CC(O)C([O-])=O.CC(O)C([O-])=O HLKMEIITONDPGG-UHFFFAOYSA-L 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
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- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 1
- 239000001527 calcium lactate Substances 0.000 description 1
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- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 1
- VNSBYDPZHCQWNB-UHFFFAOYSA-N calcium;aluminum;dioxido(oxo)silane;sodium;hydrate Chemical compound O.[Na].[Al].[Ca+2].[O-][Si]([O-])=O VNSBYDPZHCQWNB-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
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- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 description 1
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- RSAZYXZUJROYKR-UHFFFAOYSA-N indophenol Chemical compound C1=CC(O)=CC=C1N=C1C=CC(=O)C=C1 RSAZYXZUJROYKR-UHFFFAOYSA-N 0.000 description 1
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- 229940001447 lactate Drugs 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 description 1
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- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
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Abstract
【解決手段】本発明は、陽イオン交換性フィラー、陰イオン交換性フィラーおよび陽イオン交換能を有するフィラー分散剤をアルギン酸塩水溶液と混合して懸濁混合液を形成する工程、該懸濁混合液を多価金属イオン水溶液に滴下してゲル化粒子を形成する工程、および
該ゲル化粒子を水洗して、乾燥する工程を含み、該アルギン酸塩水溶液100質量部に対して、該フィラー分散剤1〜15質量部を含有することを特徴とする、陽イオン交換能および陰イオン交換能を有する粒状体の製造方法に関する。
【選択図】なし
Description
[M2+ 1−xM3+ x(OH)2]x+[An− x/n・mH2O]x− (a)
[Al2Li(OH)6]x+[An− x/n・mH2O]x−(b)
(ここで、0.1≦x≦0.4、0<m、nは1から4の自然数、M2+はMg、Ca、Mn、Fe、Co、Ni、Cu、Zn等に代表される2価の金属の少なくとも1種、M3+は、Al,Fe,Cr,Ga、In等に代表される3価の金属の少なくとも1種、An−は、OH−、Cl−、Br−、CO3 2−、NO3 2−、SO4 2−、Fe(CN)6 4−、酒石酸イオンで表わされるn価のイオン交換性アニオンの少なくとも1種である。)
で表わされる不定比化合物である層状複水酸化物(A)とゼオライト(B)を含有することを特徴とする層状複水酸化物/ゼオライト複合体が開示されている。この複合体は、陽イオン交換性および陰イオン交換性を有し、陽イオンおよび陰イオンの両方に対して高い吸着性能を有する。しかしながら、イオン吸着能は高いものの、ゼオライトをコア材料に使用するためコストが高く、製造過程で強アルカリ液を使用するため廃液処理が必要であり、連続生産が困難である。
該懸濁混合液を多価金属イオン水溶液に滴下してゲル化粒子を形成する工程、および
該ゲル化粒子を水洗して、乾燥する工程
を含み、
該アルギン酸塩水溶液100質量部に対して、該フィラー分散剤1〜15質量部を含有することを特徴とする、陽イオン交換能および陰イオン交換能を有する粒状体の製造方法に関するものである。
上記陽イオン交換性フィラーがゼオライトであり、上記フィラー分散剤がベントナイトであり、上記陰イオン交換性フィラーがハイドロタルサイトであり、上記アルギン酸塩水溶液がアルギン酸ナトリウム水溶液であり、多価金属イオン水溶液が塩化カルシウム水溶液であり;
上記アルギン酸塩水溶液100質量部に対して、上記陽イオン交換性フィラー5〜40質量部および上記陰イオン交換性フィラー5〜40質量部を含有する;
ことが望ましい。
該ゲル化粒子を水洗して、乾燥する工程
を含むことを要件とする。
(1)混合液の作製
以下の表1〜4に示した配合の材料を、家庭用ミキサー(三洋電機(株)製の「SM−L57」)を用いて3分間撹拌して、混合液を作製した。得られた混合液を、撹拌後1時間静置し、混合液の状態を目視にて観察し、その結果を同表に示す。
(注2)カサネン工業株式会社製ベントナイト「関西ベントナイト」
(注3)和光純薬工業株式会社製試薬のハイドロタルサイト
(注4)旭化成株式会社製の結晶性セルロース「セオラス」
(注5)昭和ケミカル株式会社製カオリンクレー「NK300」
(注6)HESS PUMICE PRODUCT社製シリカ「NCS‐3」
(注7)和光純薬工業株式会社製試薬のアルギン酸ナトリウム
上記のようにして得られた混合液の内、ペースト状になったものや沈殿(相分離)を形成したものは、それぞれ、次の工程で滴下できなかったり、相分離を起こして均一な混合液を滴下できなかったりしたため、懸濁液となったもののみについて、メスピペットを用いて、多価金属イオン水溶液としての5%の塩化カルシウム水溶液中へ滴下した。
(1)NH4 +吸着量
風乾させた試料2mLを50mLのファルコンチューブに入れ、1M酢酸アンモニウム溶液20mLを加え、30秒間振とう後、60分間静置し、吸引ろ過し、80%エタノール10mLにて洗浄を2回行い、瀘液は捨てる。1M塩化カリウム溶液30mLを加え、60分間振とう後、遠心分離(室温、12000rpm、2分間)した後、上清を分離し、インドフェノール法を用いて、吸着したNH4 +濃度を求める。NH4 +の濃度は富士平工業株式会社製土壌・作物体総合分析装置「SFP−3」により測定した。
風乾させた試料2mLを50mLのファルコンチューブに入れ、0.05M硝酸カルシウム溶液20mLを加え、60分間撹拌後、遠心分離(室温、10000rpm、1分間)した後、上清を分離し、アルカリ還元・ジアゾ色素法を用いて、吸着したNO3 −濃度を求める。NO3 −の濃度は富士平工業株式会社製土壌・作物体総合分析装置「SFP−3」により測定した。
容量300mLのポリエチレン製カップの底面に排水用の穴を開け、更に底に砂(粒径2〜5mm)を敷き詰め、上記カップの底面に水が溜まらないようにし、その上に粒状体200mLを入れ、ラディッシュの種1個を播種し、十分な水分を与え発芽させた後、5日間に1回の頻度で協和株式会社製の「ハイポニカ液肥(2液タイプ)」を500倍に希釈したもの30mLを養分として供給し、以下に示す評価基準によりラディッシュの生育性をN=3で評価した。
(評価基準)
○:露地栽培と同様に葉も実も生育し、生育良好
△:葉が大きくならず、実も肥大化しない
×:生育しない
Claims (3)
- 陽イオン交換性フィラー、陰イオン交換性フィラーおよび陽イオン交換能を有するフィラー分散剤をアルギン酸塩水溶液と混合して懸濁混合液を形成する工程、
該懸濁混合液を多価金属イオン水溶液に滴下してゲル化粒子を形成する工程、および
該ゲル化粒子を水洗して、乾燥する工程
を含み、
該アルギン酸塩水溶液100質量部に対して、該フィラー分散剤1〜15質量部を含有することを特徴とする、陽イオン交換能および陰イオン交換能を有する粒状体の製造方法。 - 前記陽イオン交換性フィラーがゼオライトであり、前記フィラー分散剤がベントナイトであり、前記陰イオン交換性フィラーがハイドロタルサイトであり、前記アルギン酸塩水溶液がアルギン酸ナトリウム水溶液であり、多価金属イオン水溶液が塩化カルシウム水溶液である、請求項1記載の製造方法。
- 前記アルギン酸塩水溶液100質量部に対して、前記陽イオン交換性フィラー5〜40質量部および前記陰イオン交換性フィラー5〜40質量部を含有する、請求項1記載の製造方法。
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