JP7470496B2 - 粒子状吸水性樹脂組成物 - Google Patents
粒子状吸水性樹脂組成物 Download PDFInfo
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- JP7470496B2 JP7470496B2 JP2019163909A JP2019163909A JP7470496B2 JP 7470496 B2 JP7470496 B2 JP 7470496B2 JP 2019163909 A JP2019163909 A JP 2019163909A JP 2019163909 A JP2019163909 A JP 2019163909A JP 7470496 B2 JP7470496 B2 JP 7470496B2
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- Prior art keywords
- resin composition
- silver
- polymer particles
- absorbent
- water
- Prior art date
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- 239000002250 absorbent Substances 0.000 title claims description 133
- 239000011342 resin composition Substances 0.000 title claims description 70
- 239000002245 particle Substances 0.000 claims description 127
- 229920000642 polymer Polymers 0.000 claims description 109
- 230000002745 absorbent Effects 0.000 claims description 105
- 239000000178 monomer Substances 0.000 claims description 68
- 238000006116 polymerization reaction Methods 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 43
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 37
- 238000004519 manufacturing process Methods 0.000 claims description 35
- 239000003638 chemical reducing agent Substances 0.000 claims description 31
- 239000004332 silver Substances 0.000 claims description 27
- 229910052709 silver Inorganic materials 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 25
- 229940100890 silver compound Drugs 0.000 claims description 22
- 150000003379 silver compounds Chemical class 0.000 claims description 22
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- 238000001035 drying Methods 0.000 claims description 10
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 10
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 6
- 230000000379 polymerizing effect Effects 0.000 claims description 6
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 6
- 229910001923 silver oxide Inorganic materials 0.000 claims description 5
- -1 alkali metal salts Chemical class 0.000 description 75
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- RWPGFSMJFRPDDP-UHFFFAOYSA-L potassium metabisulfite Chemical compound [K+].[K+].[O-]S(=O)S([O-])(=O)=O RWPGFSMJFRPDDP-UHFFFAOYSA-L 0.000 description 1
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- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- UVTKHPSJNFFIDG-UHFFFAOYSA-L potassium tetrathionate Chemical compound [K+].[K+].[O-]S(=O)(=O)SSS([O-])(=O)=O UVTKHPSJNFFIDG-UHFFFAOYSA-L 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012673 precipitation polymerization Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007717 redox polymerization reaction Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- VFWRGKJLLYDFBY-UHFFFAOYSA-N silver;hydrate Chemical compound O.[Ag].[Ag] VFWRGKJLLYDFBY-UHFFFAOYSA-N 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- HAEPBEMBOAIUPN-UHFFFAOYSA-L sodium tetrathionate Chemical compound O.O.[Na+].[Na+].[O-]S(=O)(=O)SSS([O-])(=O)=O HAEPBEMBOAIUPN-UHFFFAOYSA-L 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 150000004764 thiosulfuric acid derivatives Chemical class 0.000 description 1
- 238000012549 training Methods 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
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 239000003232 water-soluble binding agent Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- PENRVBJTRIYHOA-UHFFFAOYSA-L zinc dithionite Chemical compound [Zn+2].[O-]S(=O)S([O-])=O PENRVBJTRIYHOA-UHFFFAOYSA-L 0.000 description 1
- HSYFJDYGOJKZCL-UHFFFAOYSA-L zinc;sulfite Chemical compound [Zn+2].[O-]S([O-])=O HSYFJDYGOJKZCL-UHFFFAOYSA-L 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Description
銀又は銀化合物は、例えば、銀粉、塩化銀(I)、酸化銀(I)等であってよい。中でも、安全性、及びゲル安定性を高める観点から、銀粉、塩化銀(I)及び酸化銀(I)からなる群から選ばれる少なくとも1種であることが好ましい。銀又は銀化合物としては、1種を使用してもよく、2種以上を併用してもよい。
本実施形態に係る粒子状吸水性樹脂組成物に含まれる重合体粒子は、無機還元剤を含有する。本明細書において、無機還元剤とは、還元性を有する無機化合物をいう。無機還元剤は、還元性無機元素を有していればよく、具体的には、還元性の硫黄原子又は還元性のリン原子を有する化合物が挙げられ、好ましくは還元性の硫黄原子を含む化合物又は還元性のリン原子を含む水溶性化合物が挙げられる。
重合体粒子としては、例えば、エチレン性不飽和単量体を含有する単量体を重合させて得られる架橋重合体であってよい。すなわち、重合体粒子は、エチレン性不飽和単量体に由来する構造単位を有することができる。エチレン性不飽和単量体としては、水溶性エチレン性不飽和単量体を用いることができる。重合方法としては、逆相懸濁重合法、水溶液重合法、バルク重合法、沈殿重合法等が挙げられる。これらの中では、得られる粒子状吸水性樹脂組成物の良好な吸水特性の確保、及び、重合反応の制御が容易である観点から、逆相懸濁重合法又は水溶液重合法が好ましい。以下においては、エチレン性不飽和単量体を重合させる方法として、逆相懸濁重合法を例にとって説明する。
含水率=[Ww/(Ww+Ws)]×100
Ww:全重合工程の重合前の単量体水溶液に含まれる水分量から、乾燥工程等の工程により系外部に排出された水分量を差し引いた量に、無機還元剤、表面架橋剤等を混合する際に必要に応じて用いられる水分量を加えた含水ゲル状重合体の水分量。
Ws:含水ゲル状重合体を構成するエチレン性不飽和単量体、架橋剤、開始剤等の材料の仕込量から算出される固形分量。
本実施形態に係る粒子状吸水性樹脂組成物は、吸収体に好適に用いることができる。本実施形態に係る吸収体は、本実施形態に係る粒子状吸水性樹脂組成物を含有する。吸収体における粒子状吸水性樹脂組成物の含有量は、吸収体が吸収性物品に使用された際に十分な液体吸収性能を得る観点から、吸収体の1平米あたり100~1000g(すなわち100~1000g/m2)であることが好ましく、より好ましくは150~800g/m2、更に好ましくは200~700g/m2である。吸収性物品としての十分な液体吸収性能を発揮させる観点から、上記含有量は100g/m2以上であることが好ましい。ゲルブロッキング現象の発生を抑制する観点から、上記含有量は1000g/m2以下であることが好ましい。
本実施形態に係る吸収性物品は、吸収体のほかに、例えば、コアラップ、液体透過性トップシート、液体不透過性バックシートを備えていてよい。コアラップは、吸収体を保形するものである。液体透過性トップシートは、吸液対象の液体が浸入する側の最外部に配置されるものである。液体不透過性バックシートは、吸液対象の液体が浸入する側とは反対側の最外部に配置されるものである。
還流冷却器、滴下ロート、窒素ガス導入管、及び、撹拌機として翼径5cmの4枚傾斜パドル翼を2段で有する撹拌翼を備えた、内径11cm、内容積2Lの丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gを入れ、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加した。フラスコ内の混合物を撹拌しつつ80℃まで昇温することにより分散剤を溶解した。その後、形成された溶液を50℃まで冷却した。
ジエチレントリアミン5酢酸5ナトリウム水溶液を用いなかったこと、及び、2度目に共沸蒸留により系外へ抜き出す水の量を83.4g(合計量260.0g)としたこと以外は製造例1と同様にして、重合体粒子(乾燥品)220.8gを得た。重合体粒子の中位粒子径は350μmであった。
亜硫酸ナトリウム水溶液を用いなかったこと、及び、2度目に共沸蒸留により系外へ抜き出す水の量を84.8g(合計量261.4g)としたこと以外は製造例1と同様にして、重合体粒子(乾燥品)223.7gを得た。重合体粒子の中位粒子径は365μmであった。
製造例1と同様にして、含水ゲル状重合体を含むスラリーを得た。その後、125℃に設定した油浴にフラスコを浸漬し、n-ヘプタンと水との共沸蒸留により、n-ヘプタンを還流しながら、255.8gの水を系外へ抜き出した。その後、上記フラスコに表面架橋剤として2質量%のエチレングリコールジグリシジルエーテル水溶液4.42g(0.507ミリモル)を添加し、83℃で2時間保持した。
[実施例1]
製造例1により得られた重合体粒子を、重合体粒子の100質量部に対して0.5質量部の非晶質シリカ(オリエンタルシリカズコーポレーション、トクシールNP-S)とドライブレンドすることにより、非晶質シリカ及び重合体粒子を含む混合物を得た。
銀粉の添加量を0.03gに変更したこと以外は実施例1と同様にして、実施例2の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。
銀粉の代わりに塩化銀(I)(関東化学株式会社製、鹿特級、粒径300μm以下)を0.5g用いたこと以外は実施例1と同様にして、実施例3の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。
塩化銀(I)の添加量を0.03gに変更したこと以外は実施例3と同様にして、実施例4の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。
銀粉の代わりに酸化銀(I)(関東化学株式会社製、鹿特級、粒径約500μm)を0.5g用いたこと以外は実施例1と同様にして、実施例5の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。
酸化銀(I)の添加量を0.03gに変更したこと以外は実施例5と同様にして、実施例6の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。
製造例1により得られた重合体粒子の代わりに製造例2により得られた重合体粒子を用いたこと以外は実施例2と同様にして、実施例7の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は62g/gであった。
銀粉の代わりに銀担持ゼオライトとしてゼオミックHD10N(シナネンゼオミック株式会社製、合成ゼオライト、銀イオン及び亜鉛イオン含有、平均粒径1~2μm)を0.03g(銀元素添加量としては5ppm)用いたこと以外は実施例1と同様にして、実施例8の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。ゲル強度初期値は2148N/m2、ゲル強度3時間後値は2031N/m2、3時間ゲル強度変化率は5%であった。
製造例1により得られた重合体粒子の代わりに製造例3により得られた重合体粒子を用いたこと以外は実施例2と同様にして、比較例1の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。
銀粉を添加しなかったこと以外は実施例1と同様にして、比較例2の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は61g/gであった。
製造例1により得られた重合体粒子の代わりに製造例4により得られた重合体粒子を用いたこと、及び、銀粉を添加しなかったこと以外は実施例1と同様にして、比較例3の粒子状吸水性樹脂組成物を得た。得られた粒子状吸水性樹脂組成物の生理食塩水吸水量は60g/gであった。
粒子の中位粒子径は下記手順により測定した。すなわち、JIS標準篩を上から、目開き600μmの篩、目開き500μmの篩、目開き425μmの篩、目開き300μmの篩、目開き250μmの篩、目開き180μmの篩、目開き150μmの篩、及び、受け皿の順に組み合わせた。組み合わせた最上の篩に、粒子50gを入れ、ロータップ式振とう器(株式会社飯田製作所製)を用いてJIS Z 8815(1994)に準じて分級した。分級後、各篩上に残った粒子の質量を全量に対する質量百分率として算出し粒度分布を求めた。この粒度分布に関して粒子径の大きい方から順に篩上を積算することにより、篩の目開きと篩上に残った粒子の質量百分率の積算値との関係を対数確率紙にプロットした。確率紙上のプロットを直線で結ぶことにより、積算質量百分率50質量%に相当する粒子径を中位粒子径として得た。
製造例1により得られた重合体粒子中の無機還元剤(亜硫酸ナトリウム)の量を、以下の方法によって測定した。製造例1により得られた重合体粒子中の無機還元剤量は、87ppmであった。
粒子約10mgをポリプロピレン製容器に採取して秤量し、イオン交換水30mLを加え、蓋をして室温で1時間振とうした。次に、得られた抽出液をろ紙(No.7)を用いてろ過した後、イオン交換水を用いて100mLに定容してイオンクロマトグラフィー(IC)定量分析を行った。IC条件は下記のとおりとした。
IC装置:Thermo Fisher Scientific、ICS-5000
カラム:Dionex IonPac AS18-4μm(2mm×150mm)
ガードカラム:Dionex IonPac AG18-4μm(2mm×30mm)
除去システム:Dionex AERS-500(エクスターナルモード)
検出器:電気伝導度検出器
溶離液:17mM KOH水溶液(溶離液ジェネレーターEGC500を使用)
流速:0.25mL/min.
試料注入量:100μL
粒子状吸水性樹脂組成物の生理食塩水吸水量は以下の方法で測定した。500mL容のビーカーに、生理食塩水500gを量り取り、3cmのスターラーバー(リング無)で600r/minで撹拌させながら、粒子状吸水性樹脂組成物2.0gを、ママコが発生しないように分散させた。撹拌させた状態で60分間放置し、粒子状吸水性樹脂組成物中の重合体粒子を十分に膨潤させた。その後、あらかじめ目開き75μm標準篩の質量Wa(g)を測定しておき、これを用いて、上記ビーカーの内容物をろ過し、篩を水平に対して約30度の傾斜角となるように傾けた状態で、30分間放置することにより余剰の水分をろ別した。膨潤ゲルの入った篩の質量Wb(g)を測定し、以下の式により、生理食塩水吸水能を求めた。
生理食塩水の吸水量=(Wb-Wa)/2.0
実施例及び比較例で得られた粒子状吸水性樹脂組成物について、以下の方法でゲル安定性を評価した。
以下の組成の人工尿を調製した。
尿素:20.0g
塩化ナトリウム:8.0g
塩化カルシウムニ水和物:0.3g
硫酸マグネシウム七水和物:0.8g
硫酸第一鉄七水和物:0.05g
イオン交換水:970.9g
内容積100mLのビーカーに、上記人工尿49.0gを量り取り、マグネチックスターラーバー(8mmφ×30mmのリング無し)を投入し、マグネチックスターラー(iuchi社製:HS-30D)の上に配置した。引き続きマグネチックスターラーバーを600回転/分で回転するように調整した。次に、粒子状吸水性樹脂組成物1.0gを撹拌中のビーカー内に投入し、回転渦が消えて液面が水平になるまで撹拌を続け、測定試料となる膨潤ゲルを調製した。膨潤ゲルを調製した直後に、膨潤ゲルの入ったビーカーをラップ(三菱ケミカル株式会社製、ダイアラップ)で覆った。
ゲル強度は、図2に示す測定原理を有する装置を用いて測定した。図2に示す装置は、支持部50、可動台板60、可動台板60を駆動するための駆動部70、及び測定部80から構成される。支持部50において、支持台51に立てられた支柱52の上部に架台53が固定されている。支柱52には、上下に移動するように可動台板60が取り付けられている。可動台板60は、測定試料(ゲル)61を搭載することができる。架台53上にはパルスモーター71が搭載され、プーリー72を回転させることによって、ワイヤー73を介して可動台板60を上下に移動する。
3時間ゲル強度変化率(%)=[(ゲル強度初期値-ゲル強度3時間後値)/ゲル強度初期値]×100
Claims (7)
- 銀又は銀化合物、及び重合体粒子を含み、該重合体粒子が無機還元剤を含有する、粒子状吸水性樹脂組成物。
- 前記銀又は銀化合物が、銀粉、塩化銀(I)及び酸化銀(I)からなる群から選ばれる少なくとも1種である、請求項1に記載の粒子状吸水性樹脂組成物。
- 前記無機還元剤が前記重合体粒子の内部に含まれる、請求項1又は2に記載の粒子状吸水性樹脂組成物。
- 請求項1~3のいずれか一項に記載の粒子状吸水性樹脂組成物を含有する吸収体。
- 請求項4に記載の吸収体を備える吸収性物品。
- おむつである、請求項5に記載の吸収性物品。
- 水溶液中のエチレン性不飽和単量体を含有する単量体を重合することにより、含水ゲル状重合体を形成する重合工程と、
前記含水ゲル状重合体を乾燥して重合体粒子を形成する乾燥工程とを含む、吸水性樹脂粒子の製造方法であって、
前記重合工程中及び前記乾燥工程後からなる群から選択される少なくとも一つの工程で銀又は銀化合物を添加することと、
前記重合工程から前記乾燥工程中までの間に、無機還元剤を添加することとを更に含む、製造方法。
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