JP2019518821A - 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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- JP2019518821A JP2019518821A JP2018556868A JP2018556868A JP2019518821A JP 2019518821 A JP2019518821 A JP 2019518821A JP 2018556868 A JP2018556868 A JP 2018556868A JP 2018556868 A JP2018556868 A JP 2018556868A JP 2019518821 A JP2019518821 A JP 2019518821A
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- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
Description
本出願は、2017年1月24日付韓国特許出願第10−2017−0011253号に基づいた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。
少なくとも一部が中和された酸性基を有する水溶性エチレン系不飽和単量体を含む単量体組成物を内部架橋剤及び発泡剤の存在下で架橋重合して第1架橋重合体を含む含水ゲル重合体を形成する段階と、
前記含水ゲル重合体を粉砕する段階と、
前記粉砕された含水ゲル重合体を乾燥する段階と、
前記乾燥された重合体を粉砕する段階と、
前記粉砕された重合体を表面改質して高吸水性樹脂粒子を得る段階とを含み;
前記含水ゲル重合体を粉砕する段階は、円筒形紛砕機の内部に取り付けられたスクリュー型押出機を用いて前記含水ゲル重合体を複数の孔が形成された多孔板に押し出しながら、下記計算式1による20〜35(/s)のチョッピング指数の条件下で行われる、高吸水性樹脂の製造方法が提供される:
[計算式1]
チョッピング指数=ω×(TSC/A)
前記計算式1において、
ωは前記スクリュー型押出機におけるスクリューの角速度(2π×N/60s)であり、ここで、前記Nは前記スクリューの回転数(rpm)であり、
TSCは前記紛砕機に投入された前記含水ゲル重合体の固形分含有量(%)であり、
Aは前記多孔板の開口率(πr2×n/πR2)であり、ここで、前記rは前記多孔板に形成された孔の半径(mm)であり、前記nは前記多孔板に形成された孔の個数であり、前記Rは前記多孔板の半径(mm)である。
1)少なくとも一部が中和された酸性基を有する水溶性エチレン系不飽和単量体を含む単量体組成物を内部架橋剤及び発泡剤の存在下で架橋重合して第1架橋重合体を含む含水ゲル重合体を形成する段階と、
2)前記含水ゲル重合体を粉砕する段階と、
3)前記粉砕された含水ゲル重合体を乾燥する段階と、
4)前記乾燥された重合体を粉砕する段階と、
5)前記粉砕された重合体を表面改質して高吸水性樹脂粒子を得る段階とを含み;
前記含水ゲル重合体を粉砕する段階は、円筒形紛砕機の内部に取り付けられたスクリュー型押出機を用いて前記含水ゲル重合体を複数の孔が形成された多孔板に押し出しながら、下記計算式1による20〜35(/s)のチョッピング指数の条件下で行われる、高吸水性樹脂の製造方法が提供される:
[計算式1]
チョッピング指数=ω×(TSC/A)
前記計算式1において、
ωは前記スクリュー型押出機におけるスクリューの角速度(2π×N/60s)であり、ここで、前記Nは前記スクリューの回転数(rpm)であり、
TSCは前記紛砕機に投入された前記含水ゲル重合体の固形分含有量(%)であり、
Aは前記多孔板の開口率(πr2×n/πR2)であり、ここで、前記rは前記多孔板に形成された孔の半径(mm)であり、前記nは前記多孔板に形成された孔の個数であり、前記Rは前記多孔板の半径(mm)である。
[化学式1]
R1−COOM1
前記化学式1において、
R1は不飽和結合を含む炭素数2〜5のアルキルグループであり、
M1は水素原子、1価または2価金属、アンモニウム基または有機アミン塩である。
(メタ)アクリレート、エチレングリコールジ(メタ)アクリレート、ポリエチレングリコールジ(メタ)アクリレート、プロピレングリコールジ(メタ)アクリレート、ポリプロピレングリコールジ(メタ)アクリレート、ブタンジオールジ(メタ)アクリレート、ブチレングリコールジ(メタ)アクリレート、ジエチレングリコールジ(メタ)アクリレート、ヘキサンジオールジ(メタ)アクリレート、トリエチレングリコールジ(メタ)アクリレート、トリプロピレングリコールジ(メタ)アクリレート、テトラエチレングリコールジ(メタ)アクリレート、ジペンタエリスリトールペンタアクリレート、グリセリントリ(メタ)アクリレート、ペンタエリスリトールテトラアクリレート、トリアリルアミン、アリル(メタ)アクリレート、エチレングリコールジグリシジルエーテル、プロピレングリコール、グリセリン、またはエチレンカーボネートのような多官能性架橋剤が単独使用または2以上併用され得る。
onyl hydrazide)、OBSH)、p−トルエンスルホニルヒドラジド(p−toluenesulfonyl hydrazide、TSH)、ステアリン酸スクロース(sucrose stearate)、パルミチン酸スクロース(sucrose palmitate)、及びラウリン酸スクロース(sucrose laurate)からなる群より選ばれた1種以上の化合物を含み得る。
チョッピング指数=ω×(TSC/A)
前記計算式1において、
ωは前記スクリュー型押出機におけるスクリューの角速度(2π×N/60s)であり、ここで、前記Nは前記スクリューの回転数(rpm)であり、
TSCは前記紛砕機に投入された前記含水ゲル重合体の固形分含有量(%)であり、
Aは前記多孔板の開口率(πr2×n/πR2)であり、ここで、前記rは前記多孔板に形成された孔の半径(mm)であり、前記nは前記多孔板に形成された孔の個数であり、前記Rは前記多孔板の半径(mm)である。
高吸水性樹脂の製造装置としては、重合工程、含水ゲル粉砕工程、乾燥工程、粉砕工程、分級工程、表面架橋工程、冷却工程、分級工程、及び各工程を連結する輸送工程で構成される連続製造装置を用いた。
アクリル酸100重量部に内部架橋剤としてポリエチレングリコールジアクリレート(重量平均分子量:〜500g/mol)0.4重量部とヘキサンジオールジアクリレート0.1重量部、及び光開始剤としてIRGACURE 819 0.01重量部を混合して単量体溶液を製造した。次に、前記単量体溶液を定量ポンプで連続供給し、同時に24重量%水酸化ナトリウム水溶液160重量部を連続的にラインミキシングして単量体水溶液を製造した。この時、中和熱によって前記単量体水溶液の温度が約72℃以上に上昇したことを確認した後、温度が40℃に冷却することを待った。
前記段階1で得られた前記シート形態の含水ゲル重合体を3cm×3cmの大きさに切断した後、円筒形紛砕機の内部に取り付けられたスクリュー型押出機を用いて前記含水ゲルを複数の孔が形成された多孔板に押し出しながら、下記計算式1及び表1に示すチョッピング指数の条件下で粉砕(chopping)した。
チョッピング指数=ω×(TSC/A)
前記計算式1において、
ωは前記スクリュー型押出機におけるスクリューの角速度(2π×N/60s)であり、ここで、前記Nは前記スクリューの回転数(rpm)であり、
TSCは前記紛砕機に投入された前記含水ゲル重合体の固形分含有量(%)であり、
Aは前記多孔板の開口率(πr2×n/πR2)であり、ここで、前記rは前記多孔板に形成された孔の半径(mm)であり、前記nは前記多孔板に形成された孔の個数であり、前記Rは前記多孔板の半径(mm)である。
次に、前記段階2で粉砕された含水ゲル重合体を上下に風量転移が可能な乾燥機で乾燥させた。乾燥された粉の含水量が約2%以下になるように180℃のホットエア(hot air)を15分間下方から上方に流れるようにし、再び15分間上方から下方に流れるようにして前記含水ゲル重合体を均一に乾燥させた。
前記段階3で乾燥された重合体を紛砕機で粉砕した後、分級して150〜850μm大きさのベース樹脂を得た。
前記段階4で製造したベース樹脂100重量部を、水3重量部、メタノール3重量部、エチレンカーボネート0.5重量部を混合した架橋剤溶液と混合した後180℃で40分間表面架橋反応させた。そして、得られた生成物を冷却させた後、分級して粒径が150〜850μmの表面架橋された高吸水性樹脂粒子を得た。
前記実施例及び比較例で製造した各高吸水性樹脂の物性を次の方法で測定及び評価した。
走査電子顕微鏡(SEM)で高吸水性樹脂粒子を観察して、全体粒子中の発泡による凹部が粒子表面の1/3以上を占める粒子である発泡粒子(前記比率が1/3未満の場合多孔性粒子に分類)、深さ10μm以上の凹部または気孔を3個以上含む粒子である多孔性粒子、及び粉砕過程で粒子の形態変形が起きないため、滑らかな表面を有する粒子である非せん断粒子の比率を計算した。
ヨーロッパ不織布産業協会(European Disposables and Nonwovens Association、EDANA)の規格であるEDANA WSP 241.3により無荷重下吸収倍率による遠心分離保持能(CRC)を測定した。
[計算式A]
CRC(g/g)={[W2(g)−W1(g)−W0(g)]/W0(g)}
ヨーロッパ不織布産業協会(European Disposables and Nonwovens Association)の規格であるEDANA WSP 242.3の方法により加圧吸収能を測定した。
[計算式B]
AUP(g/g)=[W4(g)−W3(g)]/W0(g)
米国登録特許第5562646号のカラム54〜59に開示された方法により測定及び算出した。
蒸溜水1Lに9gの塩化ナトリウム及び0.1gのLorodac(主成分:線状炭素数12〜14のアルコールエトキシレート、CAS#68439−50−9)を溶解した水溶液を作って、高吸水性樹脂1gがこのような水溶液20gを吸収するのに所要される時間(秒)として算出及び測定した。このようなT−20の具体的な測定方法は、欧州特許公開第2535027号の13〜18頁に詳しく記載されている。
Claims (9)
- 少なくとも一部が中和された酸性基を有する水溶性エチレン系不飽和単量体を含む単量体組成物を内部架橋剤及び発泡剤の存在下で架橋重合して第1架橋重合体を含む含水ゲル重合体を形成する段階と、
前記含水ゲル重合体を粉砕する段階と、
前記粉砕された含水ゲル重合体を乾燥する段階と、
前記乾燥された重合体を粉砕する段階と、
前記粉砕された重合体を表面改質して高吸水性樹脂粒子を得る段階とを含み;
前記含水ゲル重合体を粉砕する段階は、円筒形紛砕機の内部に取り付けられたスクリュー型押出機を用いて前記含水ゲル重合体を複数の孔が形成された多孔板に押し出しながら、下記計算式1による20〜35(/s)のチョッピング指数の条件下で行われる、高吸水性樹脂の製造方法:
[計算式1]
チョッピング指数=ω×(TSC/A)
前記計算式1において、
ωは前記スクリュー型押出機におけるスクリューの角速度(2π×N/60s)であり、ここで、前記Nは前記スクリューの回転数(rpm)であり、
TSCは前記紛砕機に投入された前記含水ゲル重合体の固形分含有量(%)であり、
Aは前記多孔板の開口率(πr2×n/πR2)であり、ここで、前記rは前記多孔板に形成された孔の半径(mm)であり、前記nは前記多孔板に形成された孔の個数であり、前記Rは前記多孔板の半径(mm)である。 - 前記発泡剤は、前記単量体組成物に1000〜3000ppmで存在する、請求項1に記載の高吸水性樹脂の製造方法。
- 前記高吸水性樹脂粒子は、発泡による凹部が粒子表面の1/3以上を占める粒子である発泡粒子の比率が全体粒子数の10%以上である、請求項1に記載の高吸水性樹脂の製造方法。
- 前記高吸水性樹脂粒子は、発泡による凹部が粒子表面の1/3以上を占める粒子である発泡粒子及び表面に深さ10μm以上の凹部または気孔を3個以上含む粒子である多孔性粒子の和の比率が全体粒子数の50%以上である、請求項1に記載の高吸水性樹脂の製造方法。
- 前記高吸水性樹脂粒子は、生理食塩水(0.9重量%塩化ナトリウム水溶液)に対する30分間の遠心分離保持能(CRC)が26g/g以上であり、
生理食塩水(0.9重量%塩化ナトリウム水溶液)に対する0.7psi下で1時間の加圧吸収能(AUP)が21g/g以上であり、
生理食塩水(0.685重量%塩化ナトリウム水溶液)の流れ誘導性(SFC)が35(・10-7cm3・s/g)以上であり、
高吸水性樹脂1gが0.9重量%塩化ナトリウム及び0.01重量%炭素数12〜14のアルコールエトキシレート水溶液20gを吸収する所要時間を示すT−20が190秒以下である、請求項1に記載の高吸水性樹脂の製造方法。 - 前記内部架橋剤は、N,N´−メチレンビスアクリルアミド、トリメチロールプロパン
トリ(メタ)アクリレート、エチレングリコールジ(メタ)アクリレート、ポリエチレングリコールジ(メタ)アクリレート、プロピレングリコールジ(メタ)アクリレート、ポリプロピレングリコールジ(メタ)アクリレート、ブタンジオールジ(メタ)アクリレート、ブチレングリコールジ(メタ)アクリレート、ジエチレングリコールジ(メタ)アクリレート、ヘキサンジオールジ(メタ)アクリレート、トリエチレングリコールジ(メタ)アクリレート、トリプロピレングリコールジ(メタ)アクリレート、テトラエチレングリコールジ(メタ)アクリレート、ジペンタエリスリトールペンタアクリレート、グリセリントリ(メタ)アクリレート、ペンタエリストールテトラアクリレート、トリアリルアミン、アリル(メタ)アクリレート、エチレングリコールジグリシジルエーテル、プロピレングリコール、グリセリン、及びエチレンカーボネートからなる群より選ばれた1種以上の化合物を含む、請求項1に記載の高吸水性樹脂の製造方法。 - 前記発泡剤は、炭酸水素ナトリウム(sodium bicarbonate)、炭酸ナトリウム(sodium carbonate)、炭酸水素カリウム(potassium bicarbonate)、炭酸カリウム(potassium carbonate)、炭酸水素カルシウム(calcium bicarbonate)、炭酸カルシウム(calcium bicarbonate)、炭酸水素マグネシウム(magnesium bicarbonate)、炭酸マグネシウム(magnesium carbonate)、アゾジカルボンアミド(azodicarbonamide、ADCA)、ジニトロソペンタメチレンテトラミン(dinitroso pentamethylene tetramine、DPT)、p,p´−オキシビス(ベンゼンスルホニルヒドラジド)(p,p´−oxybis(benzenesulfonyl hydrazide)、OBSH)、p−トルエンスルホニルヒドラジド(p−toluenesulfonyl hydrazide、TSH)、ステアリン酸スクロース(sucrose stearate)、パルミチン酸スクロース(sucrose palmitate)、及びラウリン酸スクロース(sucrose laurate)からなる群より選ばれた1種以上の化合物を含む、請求項1に記載の高吸水性樹脂の製造方法。
- 前記水溶性エチレン系不飽和単量体は、アクリル酸、メタクリル酸、無水マレイン酸、フマル酸、クロトン酸、イタコン酸、2−アクリロイルエタンスルホン酸、2−メタクリロイルエタンスルホン酸、2−(メタ)アクリロイルプロパンスルホン酸、または2−(メタ)アクリルアミド−2−メチルプロパンスルホン酸の陰イオン性単量体とその塩;(メタ)アクリルアミド、N−置換(メタ)アクリレート、2−ヒドロキシエチル(メタ)アクリレート、2−ヒドロキシプロピル(メタ)アクリレート、メトキシポリエチレングリコール(メタ)アクリレートまたはポリエチレングリコール(メタ)アクリレートの非イオン系親水性含有単量体;及び(N,N)−ジメチルアミノエチル(メタ)アクリレートまたは(N,N)−ジメチルアミノプロピル(メタ)アクリルアミドのアミノ基含有不飽和単量体とその4級化物;からなる群より選ばれた1種以上の化合物を含む、請求項1に記載の高吸水性樹脂の製造方法。
- 前記高吸水性樹脂粒子は、150〜850μmの粒径を有する、請求項1に記載の高吸水性樹脂の製造方法。
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WO2018139768A1 (ko) | 2018-08-02 |
US20200164344A1 (en) | 2020-05-28 |
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