JP2006503949A - 吸水性ポリマー及び吸収性ポリマーの製造方法、複合体及び複合体の製造方法、化学製品並びに吸水性ポリマー又は複合体の使用 - Google Patents
吸水性ポリマー及び吸収性ポリマーの製造方法、複合体及び複合体の製造方法、化学製品並びに吸水性ポリマー又は複合体の使用 Download PDFInfo
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- JP2006503949A JP2006503949A JP2004545983A JP2004545983A JP2006503949A JP 2006503949 A JP2006503949 A JP 2006503949A JP 2004545983 A JP2004545983 A JP 2004545983A JP 2004545983 A JP2004545983 A JP 2004545983A JP 2006503949 A JP2006503949 A JP 2006503949A
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Images
Classifications
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
- B29B7/005—Methods for mixing in batches
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
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Abstract
【解決手段】 吸収性ポリマーの製造方法であって、複数の吸収性ポリマー粒子を液体と混合する第1の混合工程と、前記液体を前記ポリマー粒子の内部に分散させる第2の混合工程とを有し、前記第1の混合工程では、各ポリマー粒子の運動エネルギーが各ポリマー粒子間の付着エネルギーよりも大きくなる速度で前記ポリマー粒子を混合し、前記第2の混合工程では、前記第1の混合工程よりも低い速度で前記ポリマー粒子を撹拌することを特徴とする方法。
Description
(α1)0.1〜99.999重量%、好ましくは20〜98.99重量%、特に好ましくは30〜98.95重量%のエチレン性不飽和酸性基含有モノマーまたはその塩の重合物、またはプロトン化若しくは第4級化窒素を含有するエチレン性不飽和モノマー、若しくはそれらの混合物であって、少なくともエチレン性不飽和酸性基含有モノマー、好ましくはアクリル酸を含む混合物の重合物である。
(α2)0〜70重量%、好ましくは1〜60重量%、特に好ましくは1〜40重量%の、(α1)と共重合可能なエチレン性不飽和モノマーの重合物。
(α3)0.001〜10重量%、好ましくは0.01〜7重量%、特に好ましくは0.05〜5重量%の1種以上の架橋剤。
(α4)0〜30重量%、好ましくは1〜20重量%、特に好ましくは5〜10重量%の水溶性ポリマー。
(α5)0〜20重量%、好ましくは0.01〜7重量%、特に好ましくは0.05〜5重量%の1種以上の添加剤。
(A)ERT440.1−99による0.9重量%食塩水の最大吸収量が、少なくとも10〜1,000g/g、好ましくは15〜500g/g、特に好ましくは20〜300g/gである。
(B)ERT470.1−99による0.9重量%食塩水で抽出可能な部分が、ポリマー粒子の30重量%未満、好ましくは20重量%未満、特に好ましくは10重量%未満である。
(C)ERT460.1−99による嵩密度が、300〜1,000g/l、好ましくは310〜800g/l、特に好ましくは320〜700g/lである。
(D)ERT400.1−99による、1リットルの水中での、ポリマー粒子1gのpHが、4〜10、好ましくは5〜9、特に好ましくは5.5〜7.5である。
(E)ERT441.1−99によるCRC値が10〜100g/g、好ましくは15〜80g/g、特に好ましくは20〜60g/gである。
(F)ERT442.1−99による0.7psiの圧力(50g/cm2)下でのAAP値が、10〜60g/g、好ましくは15〜50g/g、特に好ましくは20〜40g/gである。
(G)ERT442.1−99による0.3psiの圧力(20g/cm2)下でのAAP値が、10〜100g/g、好ましくは15〜60g/g、特に好ましくは20〜50g/gである。
(A1)ERT442.1−99による0.7psiの圧力(50g/cm2)下でのAAP値が、10〜60g/g、好ましくは15〜50g/g、特に好ましくは20〜40g/gである。
(B1)ERT442.1−99による0.3psiの圧力(20g/cm2)下でのAAP値が、10〜100g/g、好ましくは15〜60g/g、特に好ましくは20〜50g/gである。
(C1)ERT441.1−99によるCRC値が、10〜100g/g、好ましくは15〜50g/g、特に好ましくは17〜40g/gである。
(D1)ERT442.1−99による方法で測定される0.7psiの圧力下でのAAP値の機械的応力による低下が、20%未満、特に好ましくは15%未満、さらに好ましくは10%未満である。
(E1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維、2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、上述した試験方法による最初の湿潤後の吸収時間が、53秒未満、好ましくは50秒未満、特に好ましくは46秒未満である。
(F1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維、2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、上述した試験方法による2回目の湿潤後の吸収時間が、253秒未満、好ましくは225秒未満、特に好ましくは200秒未満である。
(G1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維、2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、上述した試験方法による3回目の湿潤後の吸収時間が、475秒未満、好ましくは450秒未満、特に好ましくは400秒未満である。
(H1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維、2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、上述した試験方法による再湿潤値が、12.55g/g未満、好ましくは12g/g未満、特に好ましくは11g/g未満である。
ボールミルによるポリマー粒子の機械的処理によって生じる、0.7psiの圧力下でのERT442.1−99によるAAP値の低下を測定するために、0.7psiの圧力下でのERT442.1−99によるポリマー粒子のAAP値(AAP1)を最初に測定した。次に、これらのポリマー粒子に機械的応力によるダメージを与えた。10.0g±0.1gの超吸収体を秤量し、24個の磁器シリンダを有し、密閉された磁器容器に入れた。光接触タコメーターによって95rpmに達するように設定されたボールミル(Jarミル、US−Stoneware製)のローラーに2つの磁器容器を配置し、ボールミルを開始した。回転時間はストップウォッチによって計測し、6分経過後に終了した。次に、得られたポリマー粒子の0.7psiの圧力下におけるAAP値(AAP2)を再び測定した。AAP値の低下は以下のように定義される。
AAP値の低下(%)=100%−((AAP2/AAP1)×100)
吸収時間を測定するために、図3に断面を示す試験装置を使用した。この試験装置は、20.5cmの長さを有し、円形開口部(7)と入口パイプ(8)とを備えた半円筒部(6)を有する。試験装置の部品の全表面は滑らかである。開口部(7)の詳細図である図4に示すように、開口部(7)は、3〜4mmのメッシュサイズを有するふるい(9)を備えている。半円筒部(6)は実質的に半円形のボウル(10)に設けられている。入口パイプ(8)の開口部(7)の領域における半円筒部(6)とボウル(10)との間には、試験体(11)(複合体)が挿入されている。図5に、半円筒部(6)、開口部(7)、入口パイプ(8)の正確な寸法を示す。吸収時間の測定では、0.01の計測精度を有する天秤、試験装置に1kg±0.5gの負荷を与える重り、空圧式プランジャー、タイマー、定量分析のための90mmの円形濾紙(Schleicher & Schuell,Type 589/1,Schwarzbrand)、5ml/lの酸性フクシン原液で着色した0.9重量%塩化ナトリウム密度試験水溶液を使用した。試験対象の複合体を12cm×30cmに切断し、試験装置の半円筒部(6)とボウル(10)との間の中間に置いた。半円筒部(6)に9kgの負荷を与えた。80gの試験溶液を、20分間の間隔で3回にわたって、開口部(7)から入口パイプ(8)を介して複合体に供給した。20分間の間隔は試験溶液の添加から開始し、試験溶液は入口パイプに一度に入れた。吸収時間の測定は、試験溶液の添加から開始し、入口パイプから試験溶液が完全に漏出した時点で終了した。上述した測定を3回繰り返し、平均値を計算した。
再湿潤値を測定するために、図6,7に係る実験装置を使用した。9cmの直径を有する円形の試験片の形状の測定対象の複合体(11)を、重量を測定し、ペトリ皿(12)の中央に配置した。ビュレット(13)によって、80gの上述した試験溶液を1.8〜2.0ml/秒の流速で試験片の中央に添加した。試験溶液の添加後、40.0gの重量と9cmの直径を有する円形の濾紙スタック(14)(Schwarzbrand定量分析用濾紙、Schleicher & Schuell製Type 58971)を計量し(FT)、試験片の上面に慎重に置いた。濾紙スタック(14)に、重り(15)によって約20g/mm2で1,270gの負荷を10分間与えた。負荷を取り除いた後、試験片から濾紙スタック(14)を慎重に取り除き、再び計量した(FF)。再湿潤値はFT−FF(g)で決定される。測定は5回繰り返し、平均値を計算した。
ポリエチレングリコール(300)ジアクリレート1.50gと架橋剤としてのポリエチレングリコール(750)モノアリルエーテルアクリレート1.50gを、中和度が70モル%のアクリル酸ナトリウム水溶液(モノマー濃度:37.7%)964.515gに溶解した。溶解酸素を除去するために、プラスチック製重合容器内のモノマー溶液に、溶存酸素を除去するために、窒素を30分間吹き込んだ。ペルオキシ二硫酸ナトリウム0.3gの蒸留水10g溶液、2,2’−アゾビス−2−アミジノプロパン二塩酸塩0.1gの蒸留水10g溶液、過酸化水素35%溶液0.07gの蒸留水10g溶液、アスコルビン酸0.015gの蒸留水2g溶液を4℃で連続して添加することによって重合を開始した。最終温度(約100℃)に達した後、ゲルを肉挽き機で粉砕し、空気循環オーブン内で150℃で2時間乾燥した。乾燥体を粗く粉砕し、次いで粉末化し、次いで粒径が150〜850μmの粉末を篩い分けることによって加工用の粉末を得た(粉末A)。
粉末A50gを硫酸アルミニウム18水和物0.15gおよび水1.5gと激しく撹拌しながら混合し、次に炭酸エチレン0.3gと水0.3gの溶液と混合し、対流式オーブン内で170℃で90分間保持した(粉末B)。粉末Bは表1に示す特性を有していた。
二次架橋吸収性ポリマー200g(粉末B)を、1000rpmの混合速度で回転する高速回転MTIミキサー(MTI混合技術、Industrieanlagen GmbH、322758 Detmold:LM 1.5/5;1995年製造)(容積約1l)の回転ジャーに投入した。次に、4mlの脱イオン水をスポイトで注入した。約5〜15秒後、液体と吸収性ポリマーを均一に混合した。15分間の待ち時間後(成熟化)、Krupsドライミキサー3000を使用してレベル1(最低回転速度)で5分間にわたって第2の混合工程を行うことにより、付着していた粒子は互いに分離され、流動性を有し、凝集のない材料(粉末C)を得た。粉末Cは表2に示す特性を有していた。
複合体に対して、吸収性ポリマー(粉末BまたはC)50重量%、半処理セルロース繊維(Stora Fluff EF、スウェーデンのStora−Enzo AB製)47.5重量%、及び各50重量%のポリプロピレン(PP)とポリエチレン(PE)の二成分繊維(コア:PP、コート:PE、デンマークのFibervision A/S製)2.5重量%の混合物を、M&J装置を使用して、エアレイド法(幅:40cm、動作幅:36cm、動作設定:帯域速度:2m/分、ハンマーミルでの綿毛導入:3.6m/分、ポリマー添加率:400g/分、10g部分での二成分繊維の放出:0.7回/分)によって、複合体を形成した。この時、吸収性ポリマーを均一に添加した。その後の試験では、0.16g/cm3の密度を有する組織(1層、18g/m2)を含む目付が870g/m2の複合体を試験片として使用した。試験結果を表3に示す。
1’,1’’ 付着したポリマー粒子
2 液体
3 湿潤ポリマー粒子
4 ポリマー粒子1またはポリマー粒子1、1’若しくは1’’の速度方向
5 2つのポリマー粒子1間の付着層
6 半円筒部
7 開口部
8 入口パイプ
9 ふるい
10 ボウル
11 複合体
12 ペトリ皿
13 ビュレット
14 濾紙
15 重り
Claims (18)
- 吸収性ポリマーの製造方法であって、複数の吸収性ポリマー粒子を液体と混合する第1の混合工程と、前記液体を前記ポリマー粒子の内部に分散させる第2の混合工程とを有し、前記第1の混合工程では、各ポリマー粒子の運動エネルギーが各ポリマー粒子間の付着エネルギーよりも大きくなる速度で前記ポリマー粒子を混合し、前記第2の混合工程では、前記第1の混合工程よりも低い速度で前記ポリマー粒子を撹拌することを特徴とする方法。
- 吸収性ポリマーの製造方法であって、複数の吸収性ポリマー粒子を液体と混合する第1の混合工程と、前記液体を前記ポリマー粒子の内部に分散させる第2の混合工程とを有し、前記第1の混合工程では、媒体中での各ポリマー粒子の移動エネルギーが各ポリマー粒子間の付着エネルギーよりも大きくなる速度で前記ポリマー粒子を混合し、前記第2の混合工程では、前記第1の混合工程よりも低い速度で前記ポリマー粒子を撹拌し、前記吸収性ポリマー粒子は、前記第1の混合工程の前に表面部分において二次架橋が行われており、前記二次架橋の前にAl3+イオンを含む化合物との接触が行われていることを特徴とする方法。
- 請求項1または2において、前記第1の混合工程における前記ポリマー粒子の平均速度は、8〜80m/秒、好ましくは15〜60m/秒、特に好ましくは20〜30m/秒であり、および/または前記第2の混合工程における前記ポリマー粒子の速度は、3m/秒未満、好ましくは0.3m/秒未満、特に好ましくは0.03m/秒未満であることを特徴とする方法。
- 前記請求項のいずれかにおいて、前記第1の混合工程におけるフルード数は、1〜50、好ましくは1.5〜40、特に好ましくは1.7〜33であり、および/または前記第2の混合工程におけるフルード数は、0.001〜1、好ましくは0.01〜0.2、特に好ましくは0.08〜0.03であることを特徴とする方法。
- 前記請求項のいずれかにおいて、前記第1の混合工程では、前記ポリマー粒子は逆混合され、特に、10〜30%の逆混合が発生することを特徴とする方法。
- 前記請求項のいずれかにおいて、前記第1の混合工程の平均滞留時間は、5〜200秒、好ましくは10〜100秒、特に好ましくは20〜60秒であることを特徴とする方法。
- 前記請求項のいずれかにおいて、前記第1の混合工程時の定常圧力は、安全な混合のために、0.1バール未満、好ましくは0.05バール未満、特に好ましくは0.01バール未満であることを特徴とする方法。
- 前記請求項のいずれかにおいて、水または水溶液を前記液体として添加することを特徴とする方法。
- 請求項8において、前記液体は、添加剤、特にアルコールを含むことを特徴とする方法。
- 前記請求項のいずれかにおいて、前記ポリマー粒子は以下の成分(α1)〜(α5)((α1)〜(α5)の重量の合計は100重量%):
(α1)0.1〜99.999重量%のプロトン化若しくは第4級化窒素を含有するエチレン性不飽和モノマー、またはそれらの混合物の重合物、
(α2)0〜70重量%の(α1)と共重合可能なエチレン性不飽和モノマーの重合物、
(α3)0.001〜10重量%の1種以上の架橋剤、
(α4)0〜30重量%の水溶性ポリマー、
(α5)0〜20重量%の1種以上の添加剤、
を含むことを特徴とする方法。 - 前記請求項のいずれかにおいて、前記ポリマー粒子は、以下の特性:
(A)0.9重量%食塩水の最大吸収量が少なくとも10〜1000g/gであること、
(B)0.9重量%食塩水で抽出可能な部分がSAP粒子の30重量%未満であること、
(C)嵩密度が300〜1000g/lであること、
(D)1リットルの水中での、SAP粒子1gのpHが4〜10であること、
(E)CRC値が10〜100g/gであること、
(F)0.7psiの圧力下におけるAAP値が10〜60g/gであること、
(G)0.3psiの圧力下におけるAAP値が10〜100g/gであること、の少なくとも1つを有することを特徴とする方法。 - 前記請求項のいずれかに記載の方法によって得られる吸収性ポリマー。
- 吸収性ポリマーであって、前記吸収性ポリマーの総重量に対して0.1〜20重量%の水を含み、以下の特性:
(A1)0.7psi(50g/cm2)の圧力下におけるAAP値が10〜60g/gであること、
(B1)0.3psi(20g/cm2)の圧力下におけるAAP値が10〜100g/gであること、
(C1)CRC値が10〜100g/gであること、
(D1)機械的応力による0.7psiの圧力下におけるAAP値の低下が20%未満であること、
(E1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維及び2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、本明細書に記載する試験方法による最初の湿潤後の吸収時間が53秒未満であること、
(F1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維及び2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、本明細書に記載する試験方法による2回目の湿潤後の吸収時間が253秒未満であること、
(G1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維及び2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、本明細書に記載する試験方法による3回目の湿潤後の吸収時間が475秒未満であること、
(H1)50重量%の吸収性ポリマー、47.5重量%のセルロース繊維及び2.5重量%のポリプロピレンとポリエチレンの二成分繊維からなる複合体において、本明細書に記載する試験方法による再湿潤値が12.55g/g未満であること、の少なくとも1つを有することを特徴とする吸収性ポリマー。 - 請求項12または13に記載の吸収性ポリマーと、基材と、を含むことを特徴とする複合体。
- 複合体の製造方法であって、請求項12または13に記載の吸収性ポリマーと、基材と、必要に応じて添加剤と、を接触させることを特徴とする方法。
- 請求項15に記載の方法によって得られる複合体。
- 請求項12または13に記載の吸収性ポリマーまたは請求項14または16に記載の複合体を含むことを特徴とする化学製品。
- 請求項12または13に記載の吸収性ポリマーまたは請求項14または16に記載の複合体の、化学製品における使用。
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US7893134B2 (en) | 2011-02-22 |
CN1708541A (zh) | 2005-12-14 |
DE10249822A1 (de) | 2004-05-13 |
EP1572782B1 (de) | 2015-02-25 |
CN101058676A (zh) | 2007-10-24 |
US20090209683A1 (en) | 2009-08-20 |
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