JP7540847B2 - 高吸水性樹脂の製造方法 - Google Patents
高吸水性樹脂の製造方法 Download PDFInfo
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- JP7540847B2 JP7540847B2 JP2022574596A JP2022574596A JP7540847B2 JP 7540847 B2 JP7540847 B2 JP 7540847B2 JP 2022574596 A JP2022574596 A JP 2022574596A JP 2022574596 A JP2022574596 A JP 2022574596A JP 7540847 B2 JP7540847 B2 JP 7540847B2
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- 239000001530 fumaric acid Substances 0.000 description 1
- 238000010413 gardening Methods 0.000 description 1
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- FAIDIRVMPHBRLT-UHFFFAOYSA-N propane-1,2,3-triol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OCC(O)CO FAIDIRVMPHBRLT-UHFFFAOYSA-N 0.000 description 1
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- VPYJNCGUESNPMV-UHFFFAOYSA-N triallylamine Chemical compound C=CCN(CC=C)CC=C VPYJNCGUESNPMV-UHFFFAOYSA-N 0.000 description 1
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- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Description
本出願は2020年11月18日付韓国特許出願第10-2020-0154962号および2021年11月17日付韓国特許出願第10-2021-0158413号に基づく優先権の利益を主張し、当該韓国特許出願の文献に開示されたすべての内容は本明細書の一部として含まれる。
a)水溶性エチレン系不飽和単量体、内部架橋剤、および溶媒を混合して第1単量体混合物を製造する段階;
b)前記第1単量体混合物を剪断混合しながら、幅が3nm~50nmであり、長さが1μm~5μmであり、引張強度が2,000MPa以上のナノセルロース繊維および界面活性剤を投入して第2単量体混合物を製造する段階;
c)前記第2単量体混合物に重合開始剤を投入して第3単量体混合物を製造する段階;
d)前記第3単量体混合物を重合して含水ゲル状重合体を製造する段階;
e)前記含水ゲル状重合体をチョッピングする段階;
f)前記含水ゲル状重合体を乾燥、粉砕、および分級してベース樹脂を製造する段階;および
g)表面架橋剤の存在下で前記ベース樹脂の表面を追加架橋して表面架橋層を形成する段階;を含む高吸水性樹脂の製造方法を提供する。
前記ベース樹脂粒子の表面に形成されており、前記架橋重合体が表面架橋剤を媒介に追加架橋した表面架橋層;および
前記ベース樹脂に混入された、幅が3nm~50nmであり、長さが1μm~5μmであり、引張強度が2,000MPa以上のナノセルロース繊維を含み、
ゲル強度が10,000Pa以上である、高吸水性樹脂を提供する。
a)水溶性エチレン系不飽和単量体、内部架橋剤、および溶媒を混合して第1単量体混合物を製造する段階;
b)前記第1単量体混合物を剪断混合しながら、幅が3nm~50nmであり、長さが1μm~5μmであり、引張強度が2,000MPa以上のナノセルロース繊維および界面活性剤を投入して第2単量体混合物を製造する段階;
c)前記第2単量体混合物に重合開始剤を投入して第3単量体混合物を製造する段階;
d)前記第3単量体混合物を重合して含水ゲル状重合体を製造する段階;
e)前記含水ゲル状重合体をチョッピングする段階;
f)前記含水ゲル状重合体を乾燥、粉砕、および分級してベース樹脂を製造する段階;および
g)表面架橋剤の存在下で前記ベース樹脂の表面を追加架橋して表面架橋層を形成する段階;を含む。
実施例1
アクリル酸、苛性ソーダおよび架橋剤としてポリエチレングリコールジアクリレート(Mw=523)0.5重量%(アクリル酸100重量%に対して)を含む中和度72%、単量体濃度が43重量%である第1単量体混合物を製造した。
ナノセルロース繊維0.3%水分散液の投入量を60gに増量したことを除いては実施例1と同様の方法で高吸水性樹脂を製造した。
第1単量体混合物にナノセルロース繊維および界面活性剤を投入するとき、ホモジナイザーの剪断速度を20s-1にしたことを除いては実施例1と同様の方法で高吸水性樹脂を製造した。
アクリル酸、苛性ソーダおよび架橋剤としてポリエチレングリコールジアクリレート(Mw=523)0.5重量%(アクリル酸100重量%に対して)を含む中和度72%、単量体濃度が43重量%である第1単量体混合物を製造した。
第1単量体混合物にナノセルロース繊維および界面活性剤を投入するときホモジナイザーを用いた高剪断混合を実施しなかったことを除いては、実施例1と同様の方法で高吸水性樹脂を製造した。
幅100nm、長さ3μm、引張強度10,000MPaのナノセルロース繊維を使用したことを除いては、実施例1と同様の方法で高吸水性樹脂を製造した。
幅5nm、長さ7μm、引張強度10,000MPaのナノセルロース繊維を使用したことを除いては、実施例1と同様の方法で高吸水性樹脂を製造した。
幅5nm、長さ3μm、引張強度1,000MPaのナノセルロース繊維を使用したことを除いては、実施例1と同様の方法で高吸水性樹脂を製造した。
前記各実施例および比較例の高吸水性樹脂に対して下記方法で物性を測定し、その結果を表1に示した。
各樹脂の無荷重下吸収倍率による保水能をEDANA WSP 241.3に従って測定した。
CRC(g/g)={[W2(g)-W1(g)]/W0(g)}-1
各樹脂の0.7psiの加圧吸収能を、EDANA法WSP 242.3に従って測定した。加圧吸収能測定時には、前記CRC測定時の樹脂分級分を使用した。
0.7AUP(g/g)=[W5(g)-W4(g)]/W3(g)
JIS K 7224標準に従って測定した。より具体的には、25℃の50mLの生理食塩水に2gの高吸水性樹脂を入れ、マグネチックバー(直径8mm、長さ31.8mm)を600rpmで攪拌して渦流(vortex)が消えるまでの時間を秒単位で測定して算出した。
実施例および比較例の0.3psi加圧吸引力は韓国公開特許第10-2016-0147283号の図1に示す測定装置(X)を用いてEDANA法WSP 242.3を変形した下記の方法で測定した。
0.3吸引力(g/g)=(W7(g)-W6(g))/高吸水性樹脂の質量(0.16(g))
W6は吸水開始前の測定部4の質量(すなわち、高吸水性樹脂(0.16g)+円筒40+ナイロンメッシュ41+重り42の総質量)であり、
W7は吸水開始時点から60分経過後の測定部4の質量である。
実施例および比較例の高吸水性樹脂に対して、水平方向ゲル強度(Gel Strength)を測定した。
Claims (11)
- a)水溶性エチレン系不飽和単量体、内部架橋剤、および溶媒を混合して第1単量体混合物を製造する段階;
b)前記第1単量体混合物を剪断混合しながら、幅が3nm~50nmであり、長さが1μm~5μmであり、引張強度が2,000MPa以上のナノセルロース繊維および界面活性剤を投入して第2単量体混合物を製造する段階;
c)前記第2単量体混合物に重合開始剤を投入して第3単量体混合物を製造する段階;
d)前記第3単量体混合物を重合して含水ゲル状重合体を製造する段階;
e)前記含水ゲル状重合体をチョッピングする段階;
f)前記含水ゲル状重合体を乾燥、粉砕、および分級してベース樹脂を製造する段階;および
g)表面架橋剤の存在下で前記ベース樹脂の表面を追加架橋して表面架橋層を形成する段階;を含み、
b)段階の剪断混合は剪断速度6s -1 以上で行われる、高吸水性樹脂の製造方法。 - 前記ナノセルロース繊維は引張強度が3,000MPa~20,000MPaである、請求項1に記載の高吸水性樹脂の製造方法。
- 前記ナノセルロース繊維は水溶性エチレン系不飽和単量体100重量部に対して0.001~10重量部で含まれる、請求項1または2に記載の高吸水性樹脂の製造方法。
- 前記界面活性剤は炭素数10~30の脂肪酸ナトリウム、スルホン酸塩、またはソルビタンエステルである、請求項1から3のいずれか一項に記載の高吸水性樹脂の製造方法。
- 前記界面活性剤は水溶性エチレン系不飽和単量体100重量部に対して0.01~1重量部で含まれる、請求項1から4のいずれか一項に記載の高吸水性樹脂の製造方法。
- 水溶性エチレン系不飽和単量体が内部架橋剤の存在下で架橋重合された架橋重合体を含むベース樹脂粒子;
前記ベース樹脂粒子の表面に形成されており、前記架橋重合体が表面架橋剤を媒介に追加架橋した表面架橋層;および
前記ベース樹脂粒子に混入された、幅が3nm~50nmであり、長さが1μm~5μmであり、引張強度が2,000MPa以上のナノセルロース繊維を含み、
ゲル強度が10,000Pa以上である、高吸水性樹脂。 - 前記高吸水性樹脂は、高吸水性樹脂100重量%中のナノセルロース繊維の含有量が0.0001~10重量%である、請求項6に記載の高吸水性樹脂。
- EDANA法WSP 241.3に従って測定した遠心分離保水能(CRC)が24~45g/gである、請求項6または7に記載の高吸水性樹脂。
- EDANA法WSP 242.3に従って測定した0.7psiの加圧吸収能(AUL)が23~40g/gである、請求項6から8のいずれか一項に記載の高吸水性樹脂。
- JIS K 7224に従って測定した吸収速度(vortex time)が55秒以下である、請求項6から9のいずれか一項に記載の高吸水性樹脂。
- 0.3psiの吸引力が18g/g以上である、請求項6から10のいずれか一項に記載の高吸水性樹脂。
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