JP5777697B2 - 粗粒状の担体シリカ - Google Patents
粗粒状の担体シリカ Download PDFInfo
- Publication number
- JP5777697B2 JP5777697B2 JP2013500426A JP2013500426A JP5777697B2 JP 5777697 B2 JP5777697 B2 JP 5777697B2 JP 2013500426 A JP2013500426 A JP 2013500426A JP 2013500426 A JP2013500426 A JP 2013500426A JP 5777697 B2 JP5777697 B2 JP 5777697B2
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- JP
- Japan
- Prior art keywords
- silica
- granular
- value
- absorbent
- granular silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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Description
・0.90ml/g超のHg細孔容積(<4μm)
・3000μm未満のdQ3=90%値と同時に400μm超のdQ3=10%値
・<4.00の、3分の超音波作用後のd50値に対する超音波作用なしでのd50値の比
を有する粒状シリカである。前記測定はその際に400〜500μmの粒子の分級物で行われる。
・5〜8.5のpH値
・1.00〜3.00、好ましくは1.00〜2.60、特に好ましくは1.00〜2.10、殊に好ましくは1.00〜1.60の、3分の超音波作用後のd50値に対する超音波作用なしでのd50値の比。前記測定はその際に400〜500μmの粒子の分級物で行われる。
a)乾燥及び/又は粉砕され、
・0.1〜350μmの超音波処理なしでの平均粒度d50、
・30〜800m2/gのBET表面積、及び
・140〜400g/100gのDBP数
を有する沈降シリカ又は熱分解シリカを準備する工程;
b)工程a)からの前記シリカを、使用される成形方法に相応して30〜80質量%の乾燥減量に給湿する工程;
c)工程b)からの前記シリカを、押出し、造粒、コンパクティング、又は他の常用の成形方法により成形する工程;
d)前記シリカ成形体を、そのために適した乾燥装置中で乾燥させる工程;及び
e)前記造粒物を、3000μmのふるいサイズでスクリーン造粒又はふるい分けし、かつその細粒分を400μmのふるいの目開きでふるい分けする工程
を含む、本発明による粒状シリカの第一の製造方法である。
i)乾燥及び/又は粉砕され、<30質量%の乾燥減量を有し、かつ
・0.1〜350μmの超音波処理なしでの平均粒度d50、
・30〜800m2/gのBET表面積、及び
・140〜400g/100gのDBP数
を有する沈降シリカ又は熱分解シリカの準備する工程;
ii)工程i)からの前記シリカを、乾式コンパクティングにより、好ましくは2本の回転するロール間で、0.5kN/cmロール幅〜12kN/cmロール幅の比接触圧で、スラッグ(Stuelpen)に成形する工程、及び
iii)前記スラッグを3000μmのふるいサイズでスクリーン造粒又はふるい分けし、かつその細粒分を400μmのふるいの目開きでふるい分けする工程
を含む、本発明による粒状シリカの第二の製造方法である。
・0.1〜350μm、好ましくは0.1〜200μm、特に好ましくは0.1〜150μm及び極めて特に好ましくは1〜50μmの超音波処理なしでの平均粒度d50;
・30〜800m2/g、好ましくは40〜700m2/g、特に好ましくは50〜600m2/g、極めて特に好ましくは150〜550m2/gのBET表面積;
・140〜400g/(100g)、好ましくは140〜350g/(100g)、特に好ましくは190〜350g/(100g)、極めて特に好ましくは290〜350g/(100g)のDBP数
を有する。
BET表面積の測定
シリカの窒素比表面積(以下にBET表面積と呼ぶ)は、ISO 9277に従い、多点法表面積として測定される。測定装置としてMicromeritics社製の表面積測定装置TriStar 3000が利用される。BET表面積は通常、液体窒素の飽和蒸気圧の0.05〜0.20の分圧領域内で測定される。その試料調製は、その試料をMicromeritics社製の加熱ステーションVacPrep 061中で真空下に160℃で1時間温度調節することにより行われる。
前記シリカの吸収性の尺度であるDBP吸収量(DBP数)は、DIN 53601規格に従って次のように測定される。
DBP:DBP吸収量[g/100g]
V:DBPの消費量[ml]
D:DBPの密度[g/ml](20℃で1.047g/ml)
E:シリカの秤量分[g]
K:水分補正表による補正値[g/100g]。
シリカの水分含量が5.8%である場合には、DBP吸収量の前記のように分析された値に33g/100gの補正値Kが足される。シリカの水分は、さらに連続して本文に記載された方法"水分の測定"に従って算出される。
粉末状固体の粒度分布を測定するためのレーザー回折の使用は、粒子が、それらのサイズに応じて、単光レーザー光線の光を異なる強度パターで全ての方向へ散乱もしくは回折させるという現象に基づく。照射された粒子の直径が小さければ小さいほど、単光レーザー光線の散乱角もしくは回折角はよりいっそう大きくなる。
前記試料粒子のサイズは一部が、使用される装置の測定範囲を超え、かつ3分の超音波作用後のd50U値に対する超音波作用なしでのd50値の比は、その出発粒度に依存するので(材料のより小さい粒子は、記載されたサイズのより高い比を有する)、その測定前に400μm〜500μmの粒子分級物が前記試料からふるい分けされる。この手順により、多様な材料の安定性が確実に比較されることができ、かつ物質特異的な安定性についての証言が得られる。そのふるい分けは、400μm及び500μmふるいを備えているふるい分け機HAVER EML 200 Digital Plus、Haver & Boecker社、59302エルデを用いて行われる。出発物質5gが、上の500μmふるい上に装入され、かつ1.0の振幅設定で2分間ふるい分けされる。400μm〜500μmの粒子分級物はさらなる測定に使用される。
レーザー回折装置LS 230(Beckman Coulter社;測定範囲 0.04〜2000μm)及び液体モジュール(Small Volume Module Plus、120ml、Beckman Coulter社、一体化された超音波フィンガーあり)を用いるためのその測定のための試料調製(そのモジュールをすすぐ等)は、親水性シリカの場合に、分散液体としての脱塩水中の0.05%m/m二リン酸四ナトリウムを用いて、十分に水で湿潤可能でないシリカの場合に分散液体としてエタノール/水混合物(体積比 1:1)を用いて、行われる。
その測定の開始前に、前記レーザー回折装置は2時間ウォームアップしなければならない。その後、前記SVMモジュールは三回、前記分散液体ですすがれる。
前記粒子測定に関連した次のパラメーターが設定されるべきである:
測定時間:60秒
測定の数:1
ポンプ速度:75%
光学モデル:フラウンホーファ
PIDS機能:非作動
オフセット測定:作動
調整:自動
背景測定:作動
試料濃度を設定する:作動。
その生データ曲線から、前記ソフトウェアがフラウンホーファモデル(Fraunhofer.rfdファイル)に基づいて超音波作用なしでの粒度分布及びd50値(メジアン値)を計算する。
レーザー回折器LS 230中にあるシリカ懸濁液は、SVMモジュール中に一体化された超音波フィンガー(超音波コンバーター CV 181及び6mm超音波チップを有するSonics社製の超音波プロセッサVibra Cell VCX 130)を用い、振幅100%及び同時の液体モジュール中のポンプ循環で180秒間の超音波処理により改めて分散され、かつ前記のように測定される。
その動的画像評価の際に、バルク材料の流れは光源及びカメラの間を落ちてくる。前記粒子は、投影面積として把握され、デジタル化され、かつコンピュータプログラムを用いて粒度へ換算される。
前記粒度の測定のために、RETSCH Technology GmbH社、ハーン製のCAMSIZERが使用される。前記粒子は、貯蔵ホッパーを備えた計量供給チャネルDR 100-40を用いて前記測定装置に供給される。その画像評価のためには、共に配布されたバージョン3.12dのソフトウェアが使用されることができる。
シリカの水分は、ISO 787-2に従って測定される。このためには、1〜4gの試料量が乾燥器中で(105±2)℃で2時間乾燥され、ISOの基準に相応して評価される。この乾燥減量は主に、物理的に結合された水からなる。
前記シリカのpH値の測定は、水性懸濁液として室温で行われる。造粒された試料は、まず最初に乳鉢ですりつぶされるか又は粉砕される。シリカ5gに脱イオン水95gが添加される。前記懸濁液は、マグネチックスターラーを用いて5分間撹拌される。引き続いて直接、予想されうる測定範囲内で校正されたpH計(Metrohm 780 pH計)を用いて前記懸濁液のpH値が1の小数位で正確に測定される。
本方法は、DIN 66133による水銀圧入法に基づいており、その際にMicromeritics製のAutoPore IV 9520装置が使用される。
その方法原理は、適用される圧力に依存した、多孔質の固体へ圧入された水銀体積の測定に基づく。その際に、適用された圧力(最大414MPa)下で水銀が侵入することができる細孔のみが把握される(Ritter及びDrakeによる方法)。
p:圧力
σ:表面張力(480mN/m*)
θ:水銀の接触角(140°*)
* DIN 66133による。
Evonik Degussa GmbH社製のSIPERNAT(登録商標)50Sを、ミキサー(Somakon社、型式MP-L1)中で、シリカ100gにつき水200mlの添加下に混合し、かつ圧縮した。その際に、標準十字型混合具(Standardmischkreuz)を備え、23℃に温度調節された0.5リットル混合容器を使用した。はかり入れたシリカ15gに、2200rpmの混合速度で20秒かけて水30gを計量供給し、引き続き造粒するまで混合する。このプロセスは、外側で少し湿った5mmアグロメレートが生じると直ちに止める。得られた造粒物を乾燥器中で160℃で恒量まで乾燥させ、引き続き500μmふるいを通過させ、さらなる作業工程において400μmふるいでふるい分けする。こうして得られた400〜500μmのふるい分級物を、引き続きその硬さ及び多孔度の試験に使用する。
Evonik Degussa GmbH社製のSIPERNAT(登録商標)50Sを、ミキサー(Somakon社、型式MP-L1)中で、シリカ100gにつき水270mlの添加下に混合し、かつ圧縮した。その際に、標準十字型混合具を備え、23℃に温度調節された0.5リットル混合容器を使用した。はかり入れたシリカ15gに、2200rpmの混合速度で20秒かけて水40.5gを計量供給し、引き続き造粒するまで混合する。このプロセスは、外側で少し湿った5mmアグロメレートが生じると直ちに止める。得られた造粒物を160℃で乾燥器中で恒量まで乾燥させ、引き続き500μmふるいを通過させ、さらなる作業工程において400μmふるいでふるい分けする。こうして得られた400〜500μmのふるい分級物を、引き続きその硬さ及び多孔度の試験に使用する。
例2で製造された担体シリカの試料を110℃で16時間、水蒸気雰囲気下に貯蔵し、引き続き120℃で恒量まで後乾燥させ、引き続きその硬さ及び多孔度の試験に使用する。
約25%の固体含量を有するSIPERNAT(登録商標) 22(Evonik Degussa GmbH社製)懸濁液のろ過ケークを、予め細かくして、ドラムグラニュレーター(RWK社製)中へ添加する。20%の充填度、8rpmの回転数、90分のバッチ時間並びに120℃の加熱温度の場合に、乾いた造粒物が生じる。前記造粒物を引き続き1250μmのふるいインサートを有するスクリーングラニュレーター(Frewitt社、MG 633)中で定義された最大粒度に破壊する。無塵の生成物を得るために、その細粒分を400μmふるいでのふるい分け(Gough社、Vibrecon GV 2/1、Φ600mm)により分離する。この細粒分は、前記ろ過ケークと一緒に次の造粒バッチで併用されることができる。得られた造粒物を160℃で乾燥器中で恒量まで乾燥させ、引き続き500μmふるいを通過させ、さらなる作業工程において400μmふるいでふるい分けする。こうして得られた400〜500μmのふるい分級物を、引き続きその硬さ及び多孔度の試験に使用する。
約25%の固体含量を有するSIPERNAT(登録商標) 22(Evonik Degussa GmbH社製)懸濁液のろ過ケークを、予め細かくして、ドラムグラニュレーター(RWK社製)中へ添加する。20%の充填度、8rpmの回転数、90分のバッチ時間並びに120℃の加熱温度の場合に、乾いた造粒物が生じる。
Evonik Degussa GmbH社製のSIPERNAT(登録商標) 22を、コンパクター(Bepex社、L200/50)を用いて40kNのロールの接触力でプレスする。コンパクティングされた物を引き続き2800μmのふるいインサートを有するスクリーングラニュレーター(Frewitt社、MG 633)中で定義された最大粒度に破壊する。無塵の生成物を得るために、前記造粒のその細粒分を、400μmふるいでのふるい分け(Gough社、Vibrecon GV 2/1、Φ600mm)により分離し、かつ前記コンパクターの装入部へ返送する。その試験のために、前記造粒物を500μmふるいでふるい分けし、さらなる作業工程において400μmふるいでふるい分けする。こうして得られた400〜500μmふるい分級物を、引き続きその硬さ及び多孔度の試験を使用する。
Evonik Degussa GmbH社製のSIPERNAT(登録商標)50Sを、ミキサー(Somakon社、型式MP-L1)中で、シリカ100gにつき水233ml/の添加下に混合し、かつ圧縮した。その際に、標準十字型混合具を備え、23℃に温度調節された0.5リットル混合容器を使用した。はかり入れたシリカ15gに、2200rpmの混合速度で20秒かけて水35gを計量供給し、引き続き造粒するまで混合する。このプロセスは、外側で少し湿った5mmアグロメレートが生じると直ちに止める。得られた造粒物を160℃で乾燥器中で恒量まで乾燥させ、引き続き500μmふるいを通過させ、さらなる作業工程において400μmふるいでふるい分けする。こうして得られた400〜500μmのふるい分級物を、引き続きその硬さ及び多孔度の試験に使用する。
第2表は、技術水準の比較シリカの物理−化学的性質についての記載を含む。比較例A及びBは、Evonik Degussa GmbH社製のUltrasil(登録商標) 7000 GR及びUltrasil(登録商標) VN3 GRに相当する。比較例Cは、Rhodia Chimie社製のZeosil(登録商標) 165 GR(登録商標)である。比較例Dは、Huber社製のZeodent DP-9175である。比較例A〜Cのシリカは、自動車用タイヤ用のゴムの補強に商業的に使用される。
Claims (23)
- 粒状シリカであって、
・0.90ml/g超のHg細孔容積(<4μm)、
・3000μm未満のdQ3=90%値と同時に400μm超のdQ3=10%値、及び
・<4.00の、3分の超音波作用後のd50値に対する超音波作用なしでのd50値の比を有し、その際にその測定は400〜500μmの粒子の分級物で行われる、
粒状シリカ。 - 5〜8.5の範囲内のpH値を有する、請求項1記載の粒状シリカ。
- 1.00〜3.00の、3分の超音波作用後のd50値に対する超音波作用なしでのd50値の比を有し、その測定はその際に400〜500μmの粒子の分級物で行われる、請求項1又は2記載の粒状シリカ。
- 1.35ml/g超のHg細孔容積(<4μm)を有する、請求項1又は2記載の粒状シリカ。
- 1.80ml/g超のHg細孔容積(<4μm)を有する、請求項4記載の粒状シリカ。
- 0.9〜1.34ml/gのHg細孔容積(<4μm)を有する、請求項1又は2記載の粒状シリカ。
- 0.9ml/g〜1.30ml/gのHg細孔容積(<4μm)を有する、請求項6記載の粒状シリカ。
- 0.9ml/g〜1.20ml/gのHg細孔容積(<4μm)を有する、請求項6記載の粒状シリカ。
- 粒状シリカの製造方法であって、次の工程:
a)乾燥及び/又は粉砕され、
・0.1〜350μmの超音波処理なしでの平均粒度d50、
・30〜800m2/gのBET表面積、及び
・140〜400g/100gのDBP数
を有する沈降シリカ又は熱分解シリカを準備する工程;
b)工程a)からの前記シリカを、使用される成形方法に相応して30〜80質量%の乾燥減量に給湿する工程;
c)工程b)からの前記シリカを押出し、造粒、コンパクティング、又は他の常用の成形方法により成形する工程;
d)そのシリカ成形体をこのために適した乾燥装置中で乾燥させる工程;及び
e)その造粒物を3000μmのふるいサイズでスクリーン造粒又はふるい分けし、かつその細粒分を400μmのふるいの目開きでふるい分けする工程
を含む、粒状シリカの製造方法。 - 30〜80質量%の乾燥減量を有する水含有ろ過ケークを工程c)用の出発物質として使用する、請求項9記載の方法。
- 工程c)において工程a)からの前記シリカを高速インテンシブミキサー中で圧縮し、かつ造粒する、請求項9記載の方法。
- 粒状シリカの製造方法であって、次の工程:
i)乾燥及び/又は粉砕され、<30質量%の乾燥減量を有し、かつ
・0.1〜350μmの超音波処理なしでの平均粒度d50、
・30〜800m2/gのBET表面積、及び
・140〜400g/100gのDBP数
を有する沈降シリカ又は熱分解シリカを準備する工程;
ii)工程i)からの前記シリカを乾式コンパクティングにより、0.5kN/cmロール幅〜12kN/cmロール幅の比接触圧でスラッグに成形する工程、及び
iii)その造粒物を3000μmのふるいサイズでスクリーン造粒又はふるい分けし、かつその細粒分を400μmのふるいの目開きでふるい分けする工程
を含む、粒状シリカの製造方法。 - 400μm未満の全てのふるい分級物を分離する、請求項9から12までのいずれか1項記載の方法。
- 成形工程c)及びii)を、結合剤を供給せずに実施する、請求項9又は12記載の方法。
- 吸収質を製造するための、請求項1から8までのいずれか1項記載の粒状シリカの使用。
- 請求項1から8までのいずれか1項記載の少なくとも1種の粒状シリカを含む、吸収質。
- 少なくとも1種の触媒活性物質を含有する、請求項16記載の吸収質。
- 前記吸収される物質が、1〜70質量%の割合で施与される、請求項16又は17記載の吸収質。
- 前記活性物質又は活性物質混合物が、1〜20質量%の割合で施与される、請求項16又は17記載の吸収質。
- 請求項16から19までのいずれか1項記載の吸収質の製造方法であって、
請求項1から8までのいずれか1項記載の粒状シリカを、硬化剤又は開始剤、架橋剤、触媒、薬剤学的な作用物質及び助剤、化粧用の作用物質及び助剤、洗浄剤及び/又はケア剤、風味物質、香気物質及び芳香物質、飼料もしくは飼料添加剤、食品もしくは食品添加剤、染料及び/又は顔料、アミノ酸、酸化剤又は漂白剤、殺微生物作用を有する添加剤、農業及び林業用の化学物質及び/又はコンクリート添加剤からなる群から選択される少なくとも1種の液体と接触させる
ことを特徴とする、請求項16から19までのいずれか1項記載の吸収質の製造方法。 - 接触法における、請求項16から19までのいずれか1項記載の吸収質の使用。
- 前記接触法を、固定床反応器中で、流動層反応器中で又は前記吸収質を反応混合物中で懸濁させることにより、実施する、請求項21記載の使用。
- 前記吸収質が、触媒としての酵素を請求項1から8までのいずれか1項記載の粒状シリカ上に含有する、請求項21又は22記載の使用。
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DE102012211121A1 (de) * | 2012-06-28 | 2014-01-02 | Evonik Industries Ag | Granuläre, funktionalisierte Kieselsäure, Verfahren zu deren Herstellung und deren Verwendung |
PL2950923T3 (pl) * | 2013-02-01 | 2022-04-04 | W.R. Grace & Co. - Conn. | Porowaty żel krzemionkowy jako nośnik płynnych technologii |
US20140272012A1 (en) * | 2013-03-15 | 2014-09-18 | J.M. Huber Corporation | Silica Based Salt Solution Delivery System |
PL3055359T3 (pl) * | 2013-10-07 | 2023-08-14 | Ppg Industries Ohio, Inc. | Poddane obróbce wypełniacze, kompozycje zawierające je oraz wyroby z nich przygotowane |
WO2016171753A1 (en) * | 2015-04-22 | 2016-10-27 | The United States Of America As Represented By The Secretary Of The Navy | Insect control formulation with improved autodissemination characteristics |
RU2613917C2 (ru) * | 2015-07-06 | 2017-03-22 | Общество с ограниченной ответственностью "Эмпилс - Цинк" | Способ гранулирования порошков и оборудование для его осуществления |
DE102015216505A1 (de) | 2015-08-28 | 2017-03-02 | Wacker Chemie Ag | Silica Formkörper mit geringer thermischer Leitfähigkeit |
CN106115720B (zh) * | 2016-08-14 | 2017-07-14 | 皖西学院 | 一种利用稻壳灰制备纳米二氧化硅的方法 |
CN110337469B (zh) | 2017-02-27 | 2021-06-11 | 瓦克化学股份公司 | 用于生产疏水二氧化硅颗粒的方法 |
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FR2767071B1 (fr) | 1997-08-06 | 1999-09-10 | Rhodia Chimie Sa | Composition comprenant un liquide absorbe sur un support a base de silice precipitee |
US20010051176A1 (en) | 1997-08-06 | 2001-12-13 | Jean-Francois Viot | Composition comprising a liquid absorbed on a support based on precipitated silica |
DE19807700A1 (de) * | 1998-02-24 | 1999-08-26 | Degussa | Fällungskieselsäuregranulate |
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FR2776537B1 (fr) | 1998-03-30 | 2000-05-05 | Rhodia Chimie Sa | Composition comprenant un liquide absorbe sur un support a base de silice precipitee |
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RU2012145006A (ru) | 2014-04-27 |
BR112012024021A2 (pt) | 2016-08-30 |
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TW201206827A (en) | 2012-02-16 |
KR101770855B1 (ko) | 2017-08-23 |
EP2550095A1 (de) | 2013-01-30 |
TWI534083B (zh) | 2016-05-21 |
CN102821842A (zh) | 2012-12-12 |
BR112012024021B1 (pt) | 2018-07-24 |
US10752510B2 (en) | 2020-08-25 |
WO2011117100A1 (de) | 2011-09-29 |
ES2651742T3 (es) | 2018-01-29 |
KR20130018700A (ko) | 2013-02-25 |
US20120322893A1 (en) | 2012-12-20 |
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AR080715A1 (es) | 2012-05-02 |
RU2551858C2 (ru) | 2015-05-27 |
JP2013525239A (ja) | 2013-06-20 |
CN102821842B (zh) | 2014-11-12 |
CA2794028A1 (en) | 2011-09-29 |
EP2550095B1 (de) | 2017-10-18 |
MX2012010878A (es) | 2012-10-15 |
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