JP4459209B2 - 粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、可溶物含有量の低い高吸水性樹脂の製造方法 - Google Patents
粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、可溶物含有量の低い高吸水性樹脂の製造方法 Download PDFInfo
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- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- CYKDLUMZOVATFT-UHFFFAOYSA-N ethenyl acetate;prop-2-enoic acid Chemical compound OC(=O)C=C.CC(=O)OC=C CYKDLUMZOVATFT-UHFFFAOYSA-N 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 238000003898 horticulture Methods 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 229920001477 hydrophilic polymer Polymers 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229920002114 octoxynol-9 Polymers 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- QUANRIQJNFHVEU-UHFFFAOYSA-N oxirane;propane-1,2,3-triol Chemical compound C1CO1.OCC(O)CO QUANRIQJNFHVEU-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- 239000007870 radical polymerization initiator Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 238000010558 suspension polymerization method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Landscapes
- Absorbent Articles And Supports Therefor (AREA)
- Epoxy Resins (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
尚、本発明にて生産された吸水性樹脂の粒径はほぼ0.05から1mmである。
親水性有機溶剤として例えばメタノール、エタノール、プロパノール、イソブタノール、アセトン、メチルエーテル、エチルエーテル等が使用されているが、工業的にはメタノールを使用するのが最も便利であり好ましい。
これら界面活性剤、あるいは粘りけのある有機化合物は水溶液の型態として加えるか又は単独で加えてもよい。手頃な添加量は0.001から5重量% で、よりよい添加量は0.01から3重量% である。
本発明の製造方法は上記の如く操作環境を改良した外、製造された製品の品質も大きく引き上げられおり、特に可溶物含有量が低いものである。
200mlのビーカーに高吸水性樹脂0.5gと濃度0.9重量%の食塩水185gをそれぞれ秤量して入れてから500rpm速度の攪拌機で1時間攪拌したのち、濾紙にて高吸水性樹脂の濾過液を採取する。その濾過液20gを先に0.1NのNaOHで滴定した後再び0.1NのHclで逆滴定中和して高吸水樹脂の可溶物含有量を算出する。
1) アクリル酸1760gと水2263.7gをあらかじめ窒素置換した6000 mlのフラスコに取り、冷却しつつ攪拌下に45重量%荷性ソーダ1476.3g水溶液を滴下して中和を行なう、濃度38.6wt%のアクリル酸単量体水溶液を得た、68mol%のアクリル酸は中和ののちアクリル酸ナトリムとなる。
2) 上記部分中和されたアクリル酸単量体水溶液は0.1gの過硫酸カリウムと亜硫酸ナトリウム(重量比は1:1)に交ぜ合せてジャケット付の横筒型の予備重合反応器内に仕込み混合して予備重合反応させ、反応温度は20℃、反応時間は60分で粘度100cpの予備共重合物を得る。
3) この粘りけのある予備共重合物と1gのアゾジイソブチニトリル、0.768gのエチレングリコールトリグリシジルエーテル(n=7)をべルトコンベヤ上にのりあげ、ベルトコンベヤに備えている紫外線照射燈にて上記混合体を40秒(照射度は7.1 J/cm2)照射して架橋重合反応を行わせてゲル体を形成させる。
4) 絞り式碎切機にて2mm粒径の大きさ以下のゲル体にする。
5) 130℃で2時間ほど乾燥し、ふるいで0.1mm〜0.85mm固定粒径の粉末状高吸水樹脂を得る。
6) この高吸水性樹脂10gを取り、0.1gの硫酸アルミ粉末を加えよく混合したのち更に0.4gのエチレングリコールカボネート/水/メタノール=1:1:1の混合水溶液を加え、215℃の温度で10分間加熱処理する。
7) 冷却後の高吸水性樹脂を測定した結果、保持力は29.2 g/g、20g/ cm2圧力下の吸水倍率は29.5 g/g、49g/ cm2圧力下の吸水倍率は22.5 g/g、可溶物含有量は5.1%を示した。
1) 試験例1の操作方法と同じく、但しその予備重合反応時間は180分、420分と720分にて得られた予備重合体の粘度はおのおの370cp、1350cpと5000cpで、
2) 製品の保持力は各別に32.3 g/g、34.5 g/g、37.1 g/g、20g/cm2圧力下の吸水倍率は32.7g/g、31.5 g/g、28.7 g/g、49g/cm2圧力下の吸水倍率は24.1g/g、22.9g/g、19.8g/g、可溶物含有量は5.3%、6.1%、7.6%である。
1) 操作方法は試験例1と同じく、但しその予備重合反応温度は5℃、15℃、25℃と35℃にて得られた予備重合体の粘度はおのおの15cp、80cp、270cpと1.50cpで、
2) 製品の保持力は各別に27.1g/g、28.6g/g、31.7g/g、33.4g/g、20g/ cm2圧力下の吸水倍率は27.3g/g、28.7g/g、30.9g/g、31.5g/g、49g/ cm2圧力下の吸水倍率は18.28g/g、19.8g/g、22.8g/g、23.6g/g、可溶物含有量は2.5%、3.4%、5.2%、6.1%である。
1) 操作方法は試験例1と同じく、但しその予備重合反応開始剤は過硫酸アンモンと亜硫酸ナトリウムの混合物(重量比1:1)、過酸化水素、ジイソプロピル過酸化炭酸、2,2'―ジアゾビス(2−ホルムアミジンプロパン)ジ塩化水素化物であって;
2) 製品の保持力はおのおの30.1g/g、20.7g/g、30.5g/g、31.0g/g、20g/ cm2圧力下の吸水倍率は29.6g/g、30.3g/g、28.9g/g、31.6g/g、49g/cm2圧力下の吸水倍率は23.0g/g、22.5g/g、29.2g/g、23.6g/g、可溶物含有量は5.1%、6.2%、5.4%、5.7%である。
1) 操作方法は試験例1と同じく、但しその架橋剤(エチレングリコールトリグリシジルエーテル)はおのおのプロパントリオールポリエチレングリコールトリグリシジルエーテル、トリプロパニルアミン、とエチレングリコールジアクリレートで;
2) 製品の保持力はおのおの33.2g/g、26.5g/g、27.8g/g、20g/cm2圧力下の吸水倍率は31.3g/g、27.9g/g、28.7g/g、49g/cm2圧力下の吸水倍率は24.9g/g、22.5g/g、23.6g/g、可溶物含有量は5.7%、3.5%、3.9%である
1) 操作方法は試験例1と同じく、但しその紫外線照射時間はおのおの60秒、30秒、20秒、10秒、照度は10.2 J/cm2、5.1 J/cm2、3.5 J/cm2、1.7 J/cm2で行い;
2) 製品の保持力はおのおの27.6g/g、29.6g/g、30.2g/g、36.1g/g、20g//cm2圧力下の吸水倍率は31.3g/g、32.5g/g、30.4g/g、32.9g/g、49/cm2圧力下の吸水倍率は24.9g/g、26.3g/g、24.3g/g、19.7g/g、可溶物含有量は4.2%、6.3%、7.1%、8.1%である。
1) アクリル酸1760gと水2263.7gをあらかじめ窒素置換した6000mlのフラスコに取り冷却しつつ攪拌下に45重量%の荷性ソーダ1476.3g水溶性液を滴下して中和を行ない、濃度36.6wt%のアクリル酸単量体水溶液を得た、68mol%のアクリル酸は中和ののちアクリル酸ナトリウムとなっている。
2) 上記部分中和されたアクリル酸単量体水溶液は温度20℃左右に保持しつつ0.768gのエチレングリコールトリグリシジルエーテル(n=7)を加え。
3) 更に1.9gの過酸化水素、3gの過硫酸ナトリウムと1.0gの2,2'―アゾビス(2−ホルムアミジンプロパン)ジ塩化水素化物架橋開始剤を加えて共重合反応せしめ1時間放置してゲル状に自然形成させる。
4) 絞り碎切機にて粒径2mm以下のゲル体にある。
5) 130℃で2時間ほど乾燥し、ふるいで0.1mm〜0.85mm固定粒径の粉状高吸水性樹脂を得る。
6) この高吸水性樹脂10gを取り、0.1gの硫酸アルミ粉末を加えよく混合したのち更に0.4gのエチレングリコールカボネート/水/メタノール=1:1:1の混合水溶液を加え215℃の温度で10分間加熱処理する。
7) 冷却後の高吸水性樹脂を測定した結果、保持力は33.1g/g、20g/ cm2圧力下の吸水倍率は32.0g/g、49g/ cm2圧力下の吸水倍率は22.1g/g、可溶物含有量は12.1%であった。
Claims (7)
- 中和率が50mol%以上であるアクリル酸単量体水溶液を、熱分解型あるいは酸化還元型の予備重合反応開始剤で予備重合反応させ、粘りけのある含水ゲル状共重合体にし、
ソルビトールポリグリシジルエーテル、ポリプロパントリオールポリグリシジルエーテル、エチレングリコールジグリシジルエーテル、ポリエチレングリコールジグリシジルエーテル、又はビスプロパントリオールポリグリシジルエーテルである親水性の多価エポキシ化合物と再重合開始剤を加えたのち、紫外線を照射して再重合反応させることを特徴とする、粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、かつ可溶物含有量の低い高吸水性樹脂の製造方法。 - 前記アクリル酸単量体水溶液のアクリル酸単量体はアクリル酸、メタクリル酸、あるいは2−アクリルアミド−2−メチルプロパンスルホン酸の一種又は二種以上の混合物であることを特徴とする請求項1記載の粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、かつ可溶物含有量の低い高吸水性樹脂の製造方法。
- 熱分解型の予備重合反応開始剤が、過酸化物では過酸化水素、ジ−t―ブチル過酸化物、過酸化アミン、又は過硫酸塩(アミノ塩、アルカリ金属塩)であり、アゾ化合物では2,2'―ジアゾビス(2−ホルムアミジンプロパン)ジ塩化水素化物であり、
酸化還元型の予備重合反応開始剤が、酸性亜硫酸塩、チオ硫酸塩、アスコルビン酸、又はフェライト塩であることを特徴とする請求項1記載の粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、かつ可溶物含有量の低い高吸水性樹脂の製造方法。 - 前記予備重合反応の重合反応器は攪拌ペラのついている直立式反応槽又は横式筒型容器であることを特徴とする請求項1記載の粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、かつ可溶物含有量の低い高吸水性樹脂の製造方法。
- 前記予備重合反応の重合反応温度は5〜80℃でその反応時間は0.5〜16時間であることを特徴とする請求項1記載の粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、かつ可溶物含有量の低い高吸水性樹脂の製造方法。
- 前記紫外線を照射して再重合反応させる照射時間は30〜60秒内に行なうものであることを特徴とする請求項1記載の粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、かつ可溶物含有量の低い高吸水性樹脂の製造方法。
- 請求項1記載の粉末状で水に不溶であり、水、し尿あるいは血液を吸収し、かつ可溶物含有量の低い高吸水性樹脂の製造方法において、
さらに表面架橋剤として最後に多価アルコール、多価アミン、あるいは二個又は二個以上のエポキシ基化合物を塗布することを特徴とする方法。
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