JP5933520B2 - モノマー溶液の液滴を重合することによる吸水ポリマー粒子の製造方法 - Google Patents
モノマー溶液の液滴を重合することによる吸水ポリマー粒子の製造方法 Download PDFInfo
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- JP5933520B2 JP5933520B2 JP2013500477A JP2013500477A JP5933520B2 JP 5933520 B2 JP5933520 B2 JP 5933520B2 JP 2013500477 A JP2013500477 A JP 2013500477A JP 2013500477 A JP2013500477 A JP 2013500477A JP 5933520 B2 JP5933520 B2 JP 5933520B2
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- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920006149 polyester-amide block copolymer Polymers 0.000 description 1
- 239000004633 polyglycolic acid Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229920000656 polylysine Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000346 polystyrene-polyisoprene block-polystyrene Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 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
- 230000002265 prevention Effects 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000001454 recorded image Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003335 secondary amines Chemical group 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 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
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 description 1
- BUUPQKDIAURBJP-UHFFFAOYSA-N sulfinic acid Chemical compound OS=O BUUPQKDIAURBJP-UHFFFAOYSA-N 0.000 description 1
- 150000003455 sulfinic acids Chemical class 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- AOBORMOPSGHCAX-DGHZZKTQSA-N tocofersolan Chemical compound OCCOC(=O)CCC(=O)OC1=C(C)C(C)=C2O[C@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C AOBORMOPSGHCAX-DGHZZKTQSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 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
- PREVNTWBRWRHLS-UHFFFAOYSA-M trimethyl-[1-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].C[N+](C)(C)C(C)OC(=O)C(C)=C PREVNTWBRWRHLS-UHFFFAOYSA-M 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
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Description
吸水ポリマー粒子は、
a)酸基を有し、かつ少なくとも部分的に中和されてよい少なくとも1つのエチレン性不飽和モノマー、
b)少なくとも1つの架橋剤、
c)少なくとも1つの開始剤、
d)場合により、a)において挙げられているモノマーと共重合可能な1つ以上のエチレン性不飽和モノマー、
e)場合により、1つ以上の水溶性ポリマー、及び
f)水
を含むモノマー溶液の液滴を、周囲加熱ガス相中で重合し、そして重合チャンバーを介してガス並流を流すことによって製造され、その際、重合チャンバーを出るガスの温度は90〜150℃であり、かつ重合チャンバーの内部のガス速度は0.1〜2.5m/秒である。
モノマー溶液を、ガス相中に計量供給して、すなわちWO 2008/069639 A1及びWO 2008/086976 A1において記載されている合成を使用して、液滴を形成する。液滴は、液滴プレート(droplet plate)によって生じる。
液滴重合によって得られた吸水ポリマー粒子中の残留モノマーを、ガス蒸気の存在で熱後処理によって取り出す。残留モノマーを、比較的高温で及び比較的長い滞留時間で良好に取り出すことができる。重要なことは、ここで、吸水ポリマー粒子を乾燥しすぎないことである。過度な乾燥粒子の場合に、残留モノマーは著しく減少する。高すぎる含水率は、吸水ポリマー粒子のケーキングの傾向を増加する。吸水ポリマー粒子熱後処理中に急速に乾燥しないために、ガス流は既に蒸気を含む。
ポリマー粒子を、特性のさらなる改良のために後架橋する。
特性を改良するために、吸水ポリマー粒子を、被覆、及び/又は場合により湿らせることができる。外部後処理のために使用される内部流動床、外部流動床及び/又は外部混合器、並びに/又は分離塗工機(混合器)を、吸水ポリマー粒子の被覆のために使用することができる。さらに、冷却器及び/又は分離塗工機(乾燥器)を、後架橋した吸水ポリマー粒子の被覆/加湿のために使用することができる。捕捉挙動を制御するため、及び浸透率を改良するために適した被覆(SFC又はGBP)は、例えば、無機不活性物質、例えば水不溶性金属塩、有機ポリマー、カチオンポリマー及び多価金属カチオンである。色安定性を改良するために適した被覆は、例えば還元剤及び酸化防止剤である。粉塵結合に適した被覆は例えばポリオールである。所望でないポリマー粒子のケーキングの傾向に対して適した被覆は、例えば、ヒュームドシリカ、例えばAerosil(登録商標)200、及び界面活性剤、例えばSpan(登録商標)20である。適した被覆は、アルミニウムモノアセテート、アルミニウムスルフェート、アルミニウムラクテート、Bruggolite(登録商標)FF7及びSpan(登録商標)20である。
適した有機ポリマーは、ポリアルキルメタクリレート又は熱可塑性プラスチック、例えばポリ塩化ビニル、ポリエチレンを基礎とするロウ、ポリプロピレン、ポリミド又はポリテトラフルオロエチレンである。他の例は、スチレン−イソプレン−スチレンブロックコポリマー又はスチレン−ブタジエン−スチレンブロックコポリマーである。
第一級又は第二級アミン基、例えばポリエチレンイミン、ポリアリルアミン及びポリリシンを有する全ての多官能アミンを使用することができる。本発明による方法によって噴霧された液体は、有利には、少なくとも1つのポリアミン、例えばポリビニルアミン又は部分的に水素化されたポリビニルホルムアミドを含む。
吸水ポリマー粒子は、さらに、選択的に凝集される。凝集は、重合、熱後処理、後架橋又は被覆後に実施されうる。
本発明による方法において、熱後処理及び後架橋の工程は、1つの方法工程で組み合わせられる。かかる組合せは、最終生成物におけるあらゆる残りの後架橋剤のあらゆる基線性を有することなしに非常に反応性のある後架橋剤の使用を可能にする。低い費用要求の仕様も可能にし、かつさらに前記方法は、費用効果のある低い温度で操作ができ、変色を妨げ、かつ熱分解による最終生成物の性能特性の損失を妨げる。
1 乾性ガス入口パイプ
2 乾性ガス量測定
3 ガス分布板
4 液滴装置
5 並流噴霧乾燥器、円柱状部分
6 円錐
7 T_出口測定
8 塔排ガスパイプ
9 バグハウスフィルタ
10 換気口
11 急冷ノズル
12 凝縮塔、対向流冷却
13 熱交換器
14 ポンプ
15 ポンプ
16 水出口
17 換気口
18 排ガス出口
19 窒素入口
20 熱交換器
21 換気口
22 熱交換器
23 ノズルを介した蒸気注入
24 水負荷測定器
25 条件付き内部流動床ガス
26 内部流動床の生成物の温度測定
27 内部流動床
28 外部流動床中の生成物放出、回転弁
29 外部流動床
30 換気口
31 バグハウスフィルタに対する外部流動床の排ガス出口
32 回転弁
33 篩
34 最終生成物
35 濾過した空気の入口
36 換気口
37 熱交換器
38 ノズルを介した蒸気注入
39 水負荷測定
40 条件付き外部流動床ガス
41 静的混合器
42 静的混合器
43 開始剤供給物
44 開始剤供給物
45 モノマー供給物
46 網目構造に対する細かい粒子断片の出口
47 T_出口測定(塔円周の周りの3回測定からの平均温度)
48 液滴装置
49 開始剤供給物と予め混合したモノマー
50 噴霧乾燥塔の壁
51 液滴装置の外側のパイプ
52 液滴装置の内側のパイプ
53 液滴カセット
54 テフロンブロック
55 弁
56 開始剤供給物の入口パイプコネクタと予め混合したモノマー
57 液滴プレート
58 係数板
59 温度制御水のための流量チャネル
60 モノマー溶液のための死空間を有さない流量チャネル
61 液滴カセットのステンレス鋼ブロック
62 外部熱後処理
63 任意の被覆供給物
64 架橋剤供給物
65 熱乾燥器(後架橋)
66 冷却器
67 任意の被覆/水供給物
68 塗工機
69 被覆/水供給物。
本発明は、1つ以上の空洞を有する吸水ポリマー粒子を提供し、その際空洞は、有利には1〜50μm、より有利には2〜30μm、さらにより有利には5〜20μm、最も有利には7〜15μmの内部直径を有し、残りの粒子は内部の空洞が見えない。直径1μm未満を有する空洞は、見えない空洞として考えられる。
(A)上部の液体透過層
(B)下部の液体不透過層
(C)繊維材料5〜90質量%及び吸水ポリマー粒子10〜95質量%、有利には繊維材料20〜80質量%及び吸水ポリマー粒子20〜80質量%、より有利には繊維材料30〜75質量%及び吸水ポリマー粒子25〜70質量%、最も有利には繊維材料40〜70質量%及び吸水ポリマー粒子30〜60質量%を含む、(A)及び(B)間の液体吸収コア
(D)繊維材料80〜100質量%及び吸水ポリマー粒子0〜20質量%、有利には繊維材料85〜99.9質量%及び吸水ポリマー粒子0.01〜15質量%、より有利には繊維材料90〜99.5質量%及び吸水ポリマー粒子0.5〜10質量%、最も有利には繊維材料95〜99質量%及び吸水ポリマー粒子1〜5質量%を含む、(A)及び(C)間の任意の捕捉分布層
(E)すぐに(C)の上及び/又は下に配置させた任意の組織層、並びに
(F)他の任意の成分
から構成される。
特に記載のない限り、測定は、周囲温度23±2℃、及び相対大気湿度50±10%で実施される。吸水ポリマーは、測定前に徹底的に混合される。
食塩水流動誘導性を、EP 0 640 330 A1において記載されたように、吸水ポリマー粒子の膨張ゲル層のゲル層浸透性として測定されるが、前記特許出願における19頁及び図8において記載された装置は、ガラスフリット(40)がもはや使用されず、プランジャー(39)は、シリンダー(37)と同様のポリマー材料からなり、かつ全体の接触表面にわたって均一にそれぞれ分布された9.65mmの直径を有する21内腔を含む。測定の方法及び評価は、EP 0 640 330 A1から未装填のままである。流量は、自動に記録される。
乾燥吸水ポリマー粒子1.00g(=W1)を、25mlのガラスビーカー中に計量し、そしてガラスビーカーの基材を均一に分布する。そして0.9質量%塩化ナトリウム溶液20mlを、第二のガラスビーカー中に計量分配し、このビーカーの含有物を、第一のビーカーに急いで添加し、そしてストップウォッチをスタートする。液体表面上の反射の消失によって確認した、塩溶液の最後の滴を吸収してすぐに、ストップウォッチを止める。第二のビーカーから注入され、第一のビーカー中でポリマーによって吸収された液体の抽出量を、第二のビーカーを秤量することによって正確に測定する(=W2)。ストップウォッチで測定された吸収のために要求された時間を、tとする。表面上の液体の最後の滴の消失を、時間tと定義する。
吸水ポリマー粒子の粒子形態を、顕微鏡分析による膨張状態で調査した。吸水ポリマー粒子約100mgを、ガラスの顕微鏡スライド上に置いた。シリンジで、0.9%のNaCl水溶液を、吸水ポリマー粒子上にそれらの膨張まで置いた。溶液を、粒子によって吸収されるように絶えず再び満たした。吸水ポリマー粒子が乾燥しないように注意する。膨潤時間30分後に、スライドを、顕微鏡(Leica Macroscope Z16 APO, magnification 20x, backlighting by a Schott KL2500 LCD冷却光源、カメラLeica DFC 420、全てLeica Microsysteme Vertrieb GmbH社製; Wetzlar; Germany)下に置き、そして3つの写真を、試料の異なる部位で撮った。
自由膨張ゲル床透過性を測定するための方法は、US 2005/0256757の段落番号[0061]〜[0075]において記載されている。
吸水ポリマー粒子における残留モノマーのレベルを、EDANA推奨試験方法番号WSP 210.2−05"Residual Monomers"によって測定する。
吸水ポリマー粒子の粒子サイズ分布を、Camziser(登録商標)画像解析システム(Retsch Technology GmbH; Haan; Germany)によって測定する。
平均球形度を、100〜1000μmの粒子直径断片を使用して、Camziser(登録商標)画像解析システム(Retsch Technology GmbH; Haan; Germany)で測定する。
吸水ポリマー粒子の含水率を、EDANA推奨試験方法番号WSP 230.2−05"Moisture Content"によって測定する。
吸水ポリマー粒子の遠心保持容量を、EDANA推奨試験方法番号WSP 241.2−05"Centrifuge Retention Capacity"によって測定し、遠心保持容量のより高い値のためにティーバッグを使用した。
吸水ポリマー粒子の負荷下吸水性を、EDANA推奨試験方法番号WSP 241.2−05"Absorption Under Pressure"によって測定する。
吸水ポリマー粒子の高負荷下吸水性を、質量21.0g/cm2の代わりに質量49.2g/cm2を使用することを除いて、EDANA推奨試験方法番号WSP 241.2−05"Absorption Under Pressure"と同様に測定する。
吸水ポリマー粒子のバルク密度を、EDANA推奨試験方法番号WSP 260.2−05"Density"によって測定する。
吸水ポリマー粒子中の抽出物成分のレベルを、EDANA推奨試験方法番号WSP 270.2−05"Extractables(抽出物)"によって測定する。
ベースポリマーの製造
実施例1
方法を、図1において示されるような統合流動床(27)及び外部流動床(29)を有する並流乾燥プラント中で実施した。噴霧乾燥器(5)の円柱状部分は、高さ22m及び直径3.4mを有した。内部流動床(IFB)は、直径2.0m及び堰高さ0.4mを有した。外部流動床(EFB)は、長さ3.0m、幅0.65m及び堰高さ0.5mを有した。
CRC 33.0g/g
SFC 12×10-7cm3s/g
AUHL 24.6g/g
含水率 6.0質量%。
噴霧乾燥器(5)の円柱状部分における乾性ガスのガス速度が0.59m/sであり、かつ内腔の分離が11mmであったことを除いて、実施例1を繰り返した。噴霧乾燥の頂部中にモノマー溶液を供給するために、直径200μmを有する267個の内腔を有する3つの液滴装置を使用した。
CRC 35.0g/g
SFC 8×10-7cm3s/g
AUHL 21.6g/g
抽出物 2.1質量%
残留モノマー 616ppm
含水率 9.4質量%。
FSR 0.28g/gs。
噴霧乾燥器(5)の円柱状部分における乾性ガスのガス速度が0.59m/sであり、かつ内腔の分離が11mmであったことを除いて、実施例1を繰り返した。噴霧乾燥の頂部中にモノマー溶液を供給するために、直径200μmを有する267個の内腔を有する3つの液滴装置を使用した。
CRC 40.5g/g
AUHL 12.3g/g
抽出物 3.9質量%
残留モノマー 818ppm
含水率 9.0質量%。
実施例4
実施例1において製造された吸水ポリマー粒子800gを、加熱ジャケット(モデルM5、Gebrueder Loedige Maschinenbau GmbH(Paderborn; Germany)社製)を備えた研究室用鋤刃混合器中に置いた。後架橋剤溶液を、Denacol(登録商標)EX 512(ポリグリセロールポリグリシジルエーテル;Nagase ChemteX Corporation(Osaka;Japan)社製)0.80g、プロピレングリコール6g、及び脱イオン水12gを、ビーカー中で混合することによって製造した。混合速度450rpmで、後架橋剤溶液を、シリンジを使用して、室温で3分間にわたって吸水ポリマー粒子に滴加した。5分後に、乳酸アルミニウム溶液16g(水中で25質量%)を、2分間にわたって滴加した。そして混合器を停止し、混合容器の壁に付着した生成物を、掻き出し(そしてバルクと混合し)、そして混合を60分間150rpmで続けた。バッチを加熱し、条件付き窒素(20Nm3/h、90°、乾燥窒素1kg毎に0.24kg(蒸気))のガス流下で15分間140℃で維持した。生成物を、混合器から取り出し、そしてデシケータ中で冷却させた。そして冷却した試料を、150〜850μmで櫛分けし、そして次のように特徴付けた:
CRC 34.3g/g
SFC 51×10-7cm3s/g
AUHL 27.6g/g。
実施例4を、バッチを加熱し、条件付き窒素(20Nm3/h、90°、乾燥窒素1kg毎に0.24kg(蒸気))のガス流下で45分間140℃で維持したことを除いて繰り返した。そして冷却した生成物を、150〜850μmで櫛分けし、そして次のように特徴付けた:
CRC 32.5g/g
SFC 65×10-7cm3s/g
AUHL 26.9g/g。
実施例2において製造された吸水ポリマー粒子800gを、加熱ジャケット(モデルM5、Gebrueder Loedige Maschinenbau GmbH(Paderborn; Germany)社製)を備えた研究室用鋤刃混合器中に置いた。後架橋剤溶液を、Denacol(登録商標)EX 512(ポリグリセロールポリグリシジルエーテル;Nagase ChemteX Corporation(Osaka;Japan)社製)0.80g、プロピレングリコール6g、及び脱イオン水12gを、ビーカー中で混合することによって製造した。混合速度450rpmで、後架橋剤溶液を、シリンジを使用して、室温で3分間にわたって吸水ポリマー粒子に滴加した。そして混合器を停止し、混合容器の壁に付着した生成物を、掻き出し(そしてバルクと混合し)、そして混合を60分間150rpmで連続した。バッチを加熱し、条件付き窒素(20Nm3/h、90°、乾燥窒素1kg毎に0.24kg(蒸気))のガス流化で15分間140℃で維持した。生成物を、混合器から取り出し、そしてデシケータ中で冷却させた。そして冷却した試料を、150〜850μmで櫛分けし、そして次のように特徴付けた:
CRC 41.0g/g
AUHL 30.5g/g。
実施例6を、バッチを加熱し、条件付き窒素(20Nm3/h、90°、乾燥窒素1kg毎に0.24kg(蒸気))のガス流下で45分間140℃で維持したことを除いて繰り返した。そして冷却した生成物を、150〜850μmで櫛分けし、そして次のように特徴付けた:
CRC 39.0g/g
AUHL 29.2g/g
残留モノマーレベルを、500rpm未満であると見出した。残留後架橋剤は検出されなかった。
実施例3において製造された吸水ポリマー粒子800gを、加熱ジャケット(モデルM5、Gebrueder Loedige Maschinenbau GmbH(Paderborn; Germany)社製)を備えた研究室用鋤刃混合器中に置いた。後架橋剤溶液を、Denacol(登録商標)EX 512(ポリグリセロールポリグリシジルエーテル;Nagase ChemteX Corporation(Osaka;Japan)社製)0.80g、プロピレングリコール6g、及び脱イオン水12gを、ビーカー中で混合することによって製造した。混合速度450rpmで、後架橋剤溶液を、シリンジを使用して、室温で3分間にわたって吸水ポリマー粒子に滴加した。5分後に、乳酸アルミニウム溶液16g(水中で25質量%)を、2分間にわたって滴加した。そして混合器を停止し、混合容器の壁に付着した生成物を、掻き出し(そしてバルクと混合し)、そして混合を60分間150rpmで連続した。バッチを加熱し、条件付き窒素(20Nm3/h、90°、乾燥窒素1kg毎に0.24kg(蒸気))のガス流化で15分間115℃で維持した。生成物を、混合器から取り出し、そしてデシケータ中で冷却させた。そして冷却した試料を、150〜850μmで櫛分けし、そして次のように特徴付けた:
CRC 34.7g/g
SFC 55×10-7cm3s/g
AUHL 27.8g/g。
Claims (10)
- 以下、
a)酸基を有し、かつ少なくとも部分的に中和されてよい少なくとも1つのエチレン性不飽和モノマー、
b)少なくとも1つの架橋剤、
c)少なくとも1つの開始剤、
d)場合により、a)において挙げられているモノマーと共重合可能な1つ以上のエチレン性不飽和モノマー、
e)場合により、1つ以上の水溶性ポリマー、及び
f)水
を含むモノマー溶液の液滴を、周囲加熱ガス相中で重合し、そして重合チャンバーを介してガス並流を流すことによって(その際、重合チャンバーを出るガスの温度は90〜150℃であり、かつ重合チャンバーの内部のガス速度は0.1〜2.5m/sである)、続いて、乾性ガス1kgあたり少なくとも0.01kgの蒸気を含むガス流の存在で、少なくとも60℃の温度で、多官能エポキシド及び多官能アジリジンから選択される後架橋剤で熱後架橋することによって、吸水ポリマー粒子を製造する方法。 - 前記熱後架橋を混合器中で実施し、かつ混合器内の吸水ポリマー粒子の温度が160℃以下である、請求項1に記載の方法。
- 前記熱後架橋を、可動式混合ツールを有する混合器中で実施する、請求項2に記載の方法。
- 少なくとも1つの多官能エポキシドを後架橋剤として使用する、請求項1から3までのいずれか1項に記載の方法。
- 重合チャンバーを去るガスの温度が115〜125℃である、請求項1から4までのいずれか1項に記載の方法。
- 重合チャンバー内のガス速度が0.7〜0.9m/sである、請求項1から5までのいずれか1項に記載の方法。
- 熱後架橋されたポリマー粒子を冷却する、請求項1から6までのいずれか1項に記載の方法。
- 前記モノマーa)が、少なくとも50mol%の範囲までアクリル酸である、請求項1から7までのいずれか1項に記載の方法。
- 前記モノマーa)の酸基が、少なくとも25mol%の範囲まで中和される、請求項1から8までのいずれか1項に記載の方法。
- 前記ポリマー粒子が、少なくとも15g/gの遠心保持容量を有する、請求項1から9までのいずれか1項に記載の方法。
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