JP5905401B2 - 連続シリカ生成方法およびそれから調製したシリカ生成物 - Google Patents
連続シリカ生成方法およびそれから調製したシリカ生成物 Download PDFInfo
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- JP5905401B2 JP5905401B2 JP2012555065A JP2012555065A JP5905401B2 JP 5905401 B2 JP5905401 B2 JP 5905401B2 JP 2012555065 A JP2012555065 A JP 2012555065A JP 2012555065 A JP2012555065 A JP 2012555065A JP 5905401 B2 JP5905401 B2 JP 5905401B2
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Description
本出願は、2010年2月24日に出願された米国特許出願第12/711,321号の利益を主張し、その全ての開示内容をここに参照して援用する。
沈降シリカは、酸性化剤をアルカリ金属に加えて非晶質シリカを沈殿させることにより調製できる。生成した沈殿物を普通反応媒体からろ別し、次いで洗浄し、乾燥する。一般に、適当な粒径および粒度分布を付与するために、乾燥シリカをその後機械的に粉砕する。工業規模では、前述のステップを結合した段階的なバッチプロセスによってシリカを調製することができる。かかるプロセスが資本集約できるような設備が必要であるが、これは特に反応体が消費されていない際に遊休時間が存在する場合プロセスに非効率性をしばしばもたらす。様々な他のシリカ生成プロセスが存在する一方、これらプロセスの多くは制御および規模の拡大が困難で、多くのものはシリカが生成された後の拡張処理ステップを今なお要求する。
ここに開示するシリカ生成物を調製する連続方法は、(a)液状媒質の流れを含むループ反応領域に酸性化剤およびケイ酸アルカリ金属を連続的に供給し、ここで少なくとも酸性化剤およびケイ酸アルカリ金属の一部が反応してシリカ生成物をループ反応領域内の液状媒質に形成し;(b)前記液状媒質をループ反応領域中を連続的に再循環し;(c)前記シリカ生成物を含む液状媒質の一部をループ反応領域から連続的に取り出すことを備える。
本発明の化合物、組成物、複合体、物品、装置および/または方法を開示し、説明する前に、以下に説明する実施形態は特定の化合物、組成物、複合体、物品、装置、方法または使用に限定されず、もちろん異なるものになってもよいことが理解される。また、ここで用いる用語は、特定の実施形態を説明する目的のためだけで、限定を意図するものではない。
一実施形態では、本発明の方法は酸性化剤およびアルカリ金属ケイ酸塩を液状媒質の流れを含む連続ループ反応領域に供給する連続法であり、ここで少なくとも酸性化剤およびアルカリ金属ケイ酸塩の一部が反応してループ反応領域の液状媒質内シリカ生成物を形成する。酸性化剤およびアルカリ金属ケイ酸塩を連続ループ反応領域に供給すると、ループ反応領域内の内容物(すなわち液状媒質)が連続的に再循環される。シリカ生成物は、シリカ生成物を含む液状媒質の一部を取り出すことにより回収され、一実施形態ではループ反応領域内に加えた原材料の体積に等しい。
様々な種類のシリカ生成物が、出発材料および処理条件に応じてここに開示した方法を用いて調製することができる。一実施形態では、本発明のシリカ生成物が100cc/100gまでの吸油量を有するシリカ粒子である。かかる実施形態では、シリカ粒子の少なくとも80%が丸々としたものに丸められている。これらシリカ粒子はまた、0.9よりも大きな球形度(S80)因子および100,000回転当たり8.0mgの減量未満のブラス・アインレーナー摩耗値を有する。
本発明のシリカ生成物は、特に研磨剤や洗浄剤の一部または全部として歯磨剤組成物に有用である。ここで用いる「歯磨剤組成物」は、例えば歯の接触可能表面を洗浄することにより腔衛生を維持するのに使用し得る組成物を指す。歯磨剤組成物は、液体、粉末またはペーストとすることができる。一般に、歯磨剤組成は主として水、洗浄剤、保湿剤、結合剤、香味剤および微粉砕したパウダー状研磨剤(開示したシリカ生成物)からなる。本発明のシリカ粒子は、歯磨剤組成物に組み込まれると、約5〜50質量%、好ましくは約10〜50質量%、より好ましくは約10〜35質量%のレベルで存在することができる。具体例として、歯磨剤組成物は、約20質量%で存在するシリカ粒子を含むことができる。
本発明の方法は、種々の実施形態において、連続ループ反応器または管状反応器を用いて行うことができる。適当な連続ループ反応器は、一般に一つ以上のパイプにより画定した連続ループと全て流体連結する酸性化剤用入り口と、ケイ酸アルカリ金属用入り口と、生成物の取り出し口とを備える。連続ループ内の液状媒質を、ループ自体の中にあるポンプのような種々の手段を用いて再循環する。連続ループ反応器の他の構成要素は、限定しないが、液状媒質の温度を制御するためのループ内の熱交換器、圧力制御のための背圧弁および/または液体反応媒質の内容物を混合するためのループ内のインライン混合装置を含むことができる。
以下の実施例は、当該分野の当業者に、ここに請求する化合物、組成物、物品、装置および/または方法がいかになされ、評価されるかの、完全な開示および説明を提供するために提供され、純粋に本発明の実施形態を意図したもので、本発明者らが発明とみなす範囲を限定することを意図するものではない。使用する数字(例えば、量、温度など)に関して正確性を確保するための努力はしてきたが、誤差や偏差はありうる。特に断りのない限り、部は重量部であり、温度は摂氏または室温であり、圧力は大気圧であるかそれに近い圧力である。
連続ループ反応器は、反応スラリを取り出す前に何回も循環できる再循環ループで設計された(図1参照)。再循環ループは、可撓性ホースの部分により一緒に結合された固定パイプの部分からなる。パイプ/ホースの内径はおよそ1インチとした。ループの片側にポンプを配置して反応物を循環し、反対側にSILVERSONのインラインミキサーを設けて系に付加的な剪断を付与し、また酸性化剤を導入するための入り口として用いる。ポンプとミキサーとの間に静的ミキサー熱交換器(Chemineer, Inc., Dayton, Ohioから入手可能なKENICS Model 1−Pilot−HT−EX 32)を設けてシリカの生成中に温度制御手段をもたらした。酸性化剤入り口の後に位置する取り出しパイプにより、ケイ酸塩および酸性化剤を添加する速度の関数として生成物を取り出しことが可能となる。取り出しパイプはまた、反応系を100℃超の温度で作動可能とする背圧弁を備えることができる。生成物の取り出しパイプは、生成物を追加修正(例えばpH調整)用のタンクに収集するように指向させるか、または生成物をロータリー型またはプレス型ろ過器に直接取り出すことができる。生成物を7.0超のpHで調製するときに、酸を生成物取り出しラインに任意選択的に加えて合成後のpH調整を避けることができる。
シリカ生成物を、実施例1に記載した連続ループ反応器を用いて調製した。酸性化剤およびケイ酸アルカリ金属を連続ループ反応器に導入するに先立って、沈降シリカ、硫酸ナトリウム、ケイ酸ナトリウムおよび水を先ず加え、80L/minで再循環する。これは、ここで液体反応媒質を指し、上述したとおりこれに酸性化剤およびケイ酸アルカリ金属をさらに加えることができる。この最初のステップを行って再循環ループを典型的なバッチの近似的な含有量および濃度で満たし、これにより所望のシリカ生成物を収集する前にパージ時間を最小化する。このステップはまた、ループ反応器内容物のゲル化を最小化する信じられている。しかしながら、系をゲル化または塞ぐことなしに、水だけを充填したループ反応器に酸性化剤およびケイ酸アルカリ金属を直接加えることができることに注目すべきである。したがって、液体反応媒質は、酸性化剤およびケイ酸アルカリ金属の導入に先んじて、種シリカなしで水を含むことができる。
実施例2で調製したシリカ生成物を特徴付けた。最も試験した反応条件下での反応スラリ粒径(再循環ループ内の粒子の粒径)は、一般に4〜8μmであり、最も多い例では4〜6μmに収まる。粒子の乾燥粒径および球形度/丸みは、シリカの構造に直接関係する。構造が低いと、スラリ粒径分布からの変化がほとんど無い高い球形度および丸みを有するより高い割合の非塊状粒子が乾燥により生じた。構造が高くなると、粒子凝集レベルが増加し、粒子の球形度および丸みが減少し、平均粒径が乾燥により増加する。
(i)4A
1.5kgのZEODENT103と、1.34kgの硫酸ナトリウムと、11.1Lのケイ酸ナトリウム(2.65MR、13.3%)と、20Lの水とからなる溶液を調製した。次いで、この溶液約15.5Lを実施例1に記載したループ反応器の再循環ループに加え、50℃に加熱した。60Hz(3485RPM)で作動する再循環ループ内のSILVERSONインラインミキサーを用いて、内容物を78L/分で再循環した。ケイ酸ナトリウム(2.65MR、13.3%)および二酸化炭素(99.9%)をループに同時に0.5L/分のケイ酸塩速度で、またpH9.3を維持するのに十分な二酸化炭素速度(およそ47L/分の流速)で加えた。所要に応じて、二酸化炭素速度を調整して上記pHを維持した。所望の材料を収集する前に、系から不要なシリカを除外するためにこれら状況下で二酸化炭素およびケイ酸塩を40分間加えた。40分経過後、収集容器を空にし、内容物を取り出した。温度をおよそ50℃で維持しながら40RPMの撹拌でシリカ生成物を容器に収集する間、二酸化炭素およびケイ酸塩を連続的に加えた。所望量の生成物を収集した後、二酸化炭素およびケイ酸塩の添加を止めた。ループの内容物を循環できた。収集容器のシリカ生成物を硫酸の手動付加添加でpH6.0に調節し、次いでおよそ1500μSの導電率でろ過、洗浄し、その後乾燥し、必要に応じて製粉した。
試料4Bは、ケイ酸ナトリウムが10重量%の硫酸ナトリウムを含有し、8.5のpHを維持されおよそ64L/分の二酸化炭素流速で維持した以外試料4Aの方法に従って得た。
1.5kgのZEODENT103と、1.34kgの硫酸ナトリウムと、11.1Lのケイ酸ナトリウム(2.65MR、13.3%)と、20Lの水とからなる溶液を調製した。この溶液約15.5Lをループ反応器の再循環ループに加え、43℃に加熱した。60Hz(3485RPM)で作動する再循環ループ内のSILVERSONインラインミキサーを用いて、内容物を80L/分で再循環した。ケイ酸ナトリウム(2.65MR、13.3%)と、23g/Lの濃度の硫酸ナトリウムを含む硫酸(11.4%)とをループに同時に2.55L/分のケイ酸塩速度で、かつpH7.5を維持するに十分な酸速度で加えた。所要に応じて、酸速度を調節して上記pHを維持した。所望のシリカ材料を収集する前に、系から不要なシリカを除外するためにこれら状況下で酸(硫酸ナトリウムを含有する)およびケイ酸塩を40分間加えた。40分経過後、収集容器を空にし、内容物を取り出した。温度をおよそ45℃に維持しながら40RPMの撹拌でシリカ生成物を容器に収集する間、酸(硫酸ナトリウムを含有する)およびケイ酸塩を連続的に加えた。所望量の生成物を収集した後、酸およびケイ酸塩の添加を止めた。ループの内容物は循環できた。次いで、収集容器のシリカ生成物をおよそ1500μSの導電率でろ過、洗浄した。噴霧乾燥に先んじて、pHを硫酸の手動添加で6.0に調節した。
試料4Dは、ケイ酸塩速度が1.7L/分で、pHを7.1で維持し、反応温度が95℃で、収集温度を約90℃で維持した以外、試料4Cに従って得た。
試料4Eは、ケイ酸塩濃度が19.5%で、17%の硫酸が8.5g/Lの濃度の硫酸アルミニウムを含有し、反応温度が40℃で、pHを7.5で維持した以外、試料5Dに従って得た。
開示したシリカ粒子を含む歯磨剤組成物を調製した。歯磨剤組成物に有用なシリカ生成物のいくつかの重要な特性を評価した。開示した連続法により生成した典型的なシリカ粒子のアインレーナー摩耗値は予測よりも著しく低く、1.8〜8.1mg損失/100k回転の範囲であった。従来の沈降シリカ生成物では、構造が低いので、アインレーナー値は通常増加する。開示した連続法によるシリカ生成物では、この傾向は観測されなかった。アインレーナー値は粒径と一致した。試験した典型的なシリカ生成物のパースペクス(Perspex)摩耗値も、予測よりずっと低く、3.3〜8.7の範囲であった。
(i)6A
1.5kgのZEODENT103と、1.34kgの硫酸ナトリウムと、11.1Lのケイ酸ナトリウム(3.32MR,20.0%)と、20Lの水とからなる溶液を調製した。次いで、この溶液およそ15.5Lを実施例1に記載したループ反応器の再循環ループに加え、60℃に加熱した。60Hz(3485RPM)で作動する再循環ループ内のSILVERSONインラインミキサーを用いて、内容物を80L/分で再循環した。硫酸ナトリウム(3.32MR,20.0%)および硫酸アルミニウム溶液(11.4%)をループに同時に1.7L/分のケイ酸塩の速度およびpH8.5を維持するに十分な硫酸アルミニウムの速度で加えた。所要に応じて、酸の速度を調節して上記pHを維持した。所望の材料を収集する前に、不要なシリカを系からパージするためにこれら状況下で酸およびケイ酸塩を40分間加えた。40分経過後、収集容器を空にし、その中身を取り出した。温度を約60℃で維持しながら40RPMで撹拌してケイ酸塩生成物を容器に収集する間、酸および硫酸アルミニウムを連続的に加えた。所望量の生成物を収集した後、硫酸アルミニウムおよびケイ酸塩の添加を止めた。ループの内容物は循環することできた。次いで、収集容器のケイ酸塩生成物を約1500μSの導電率でろ過、洗浄し、その後乾燥した。
実施例6Bは、再循環速度が77L/分で、反応温度が36℃で、収集容器の温度を室温で保持した以外、実施例6Aに従って行った。試料を乾燥後にレイモンド製粉した。
実施例6Cは、静的ミキサー熱交換器を装置から取り除き、反応温度を32℃とした以外、実施例6Bに従って行った。
実施例6Dは、水性硫酸アルミニウム濃度が14.5%で、ケイ酸塩の速度が3.4L/分で、反応温度が24℃である以外、実施例6Cに従って行った。
静的ミキサー熱交換器をループ反応器から取り除いた。1.5kgのZEODENT103と、1.34kgの硫酸ナトリウムと、11.1Lのケイ酸ナトリウム(3.32MR,20.0%)と、20Lの水とからなる溶液を調製した。この溶液およそ15.5Lをループ反応器の再循環ループに加え、39℃に加熱した。60Hz(3485RPM)で作動する再循環ループ内のSILVERSONインラインミキサーを用いて、内容物を110L/分で再循環した。4.5g/Lの水酸化マグネシウムを含むケイ酸ナトリウム(3.32MR,20.0%)および水性硫酸アルミニウム(34.0%)をループに同時に2.5L/分のケイ酸塩速度およびpH8.8を維持するに十分な水性硫酸アルミニウム速度で加えた。所要に応じて、水性硫酸アルミニウム速度を調節して上記pHを維持した。所望の材料を収集する前に、不要なシリカを系からパージするためにこれら状況下で水性硫酸アルミニウムおよび水酸化マグネシウムを含むケイ酸塩を25分間加えた。25分経過後、収集容器を空にし、その中身を取り出した。温度を約39℃で維持しながら40RPMで撹拌してケイ酸塩生成物を容器から収集する間、水性硫酸アルミニウムおよび水酸化マグネシウムを含むケイ酸塩を連続的に加えた。所望量の生成物を収集した後、水性硫酸アルミニウムおよび水酸化マグネシウムを含むケイ酸塩の添加を止めた。ループの内容物は循環できた。次いで、収集容器のケイ酸塩生成物を約1500μSの導電率でろ過、洗浄し、その後乾燥した。
以下、出願当初の特許請求の範囲を付記する。
[付記1]
(a)酸性化剤およびケイ酸アルカリ金属を液状媒質の流れを含むループ反応領域に連続的に供給し、ここで前記酸性化剤およびケイ酸アルカリ金属の少なくとも一部が反応してシリカ生成物を前記ループ反応領域の液状媒質に形成し、
(b)前記液状媒質を前記ループ反応領域を経て連続的に再循環し、
(c)前記シリカ生成物を含む液状媒質の一部を前記ループ反応領域から連続的に取り出すことを備えるシリカ生成物を調製する連続方法。
[付記2]
前記(a)〜(c)のステップを同時に行う上記[付記1]に記載の方法。
[付記3]
前記ループ反応領域から取り出す液状媒質の一部を、前記ループ反応領域に供給する酸性化剤およびケイ酸アルカリ金属の量に比例する量で取り出す上記[付記1]に記載の方法。
[付記4]
前記ループ反応領域から取り出す液状媒質の一部を、前記ループ反応領域に供給する酸性化剤およびケイ酸アルカリ金属の速度に比例する速度で取り出す上記[付記1]に記載の方法。
[付記5]
前記酸性化剤およびケイ酸アルカリ金属を、前記ループ反応領域に沿った異なる点で該ループ反応領域に供給する上記[付記1]に記載の方法。
[付記6]
前記液状媒質を前記反応領域を経て少なくとも15L/分の速度で再循環する上記[付記1]に記載の方法。
[付記7]
前記ケイ酸アルカリ金属を前記ループ反応領域に少なくとも0.5L/分の速度で供給する上記[付記1]に記載の方法。
[付記8]
前記酸性化剤を前記ループ反応領域に、前記液状媒質内で2.5〜10.5のpHを維持するに十分な速度で供給する上記[付記1]に記載の方法。
[付記9]
前記酸性化剤を前記ループ反応領域に、前記液状媒質内で7.0〜10.0のpHを維持するに十分な速度で供給する上記[付記1]に記載の方法。
[付記10]
前記シリカ生成物を含む液状媒質を、前記ループ反応領域から取り出すに先立って前記ループ反応領域を経て10〜200回再循環する上記[付記1]に記載の方法。
[付記11]
前記方法を連続ループ反応器内で行う上記[付記1]に記載の方法。
[付記12]
最大100cc/100gの吸油量値を有するシリカ粒子であって、該シリカ粒子の少なくとも80%を丸々としたものに丸め、0.9超の球形度(S 80 )因子および8.0mg損失/100,000回転未満のブラス・アインレーナー摩耗値を有するシリカ粒子。
[付記13]
前記シリカ粒子は、3〜15μmのメジアン粒径を有する上記[付記12]に記載のシリカ粒子。
[付記14]
前記シリカ粒子は、3〜10μmのメジアン粒径を有する上記[付記12]に記載のシリカ粒子。
[付記15]
前記シリカ粒子は、30〜80cc/100gの吸油量値を有する上記[付記12]に記載のシリカ粒子。
[付記16]
前記シリカ粒子は、50〜350m 2 /gのBET表面積を有する上記[付記12]に記載のシリカ粒子。
[付記17]
3〜15μmの粒径と、100cc/100g超の吸油量値と、20%のシリカ装填で少なくとも85の外被清浄比(PCR)値を有するシリカ粒子。
[付記18]
前記シリカ粒子は、3〜10μmのメジアン粒径を有する上記[付記17]に記載のシリカ粒子。
[付記19]
前記シリカ粒子は、100cc/100g超で150cc/100gまでの吸油量値を有する上記[付記17]に記載のシリカ粒子。
[付記20]
前記シリカ粒子は、20%装填で85〜120の外被清浄比(PCR)値を有する上記[付記17]に記載のシリカ粒子。
[付記21]
前記シリカ粒子は、50〜350m 2 /gのBET表面積を有する上記[付記17]に記載のシリカ粒子。
[付記22]
シリカ粒子を組成物の5〜50重量%の量で含む歯磨剤組成物であって、前記シリカ粒子が100cc/100gまでの吸油量値と、0.9超の球形度(S 80 )因子と、8.0mg損失/100,000回転未満のブラス・アインレーナー摩耗値とを有し、シリカ粒子の少なくとも80%が丸々としたものに丸められた歯磨剤組成物。
[付記23]
前記組成物は、保湿剤、溶媒、結合剤、治療薬、キレート剤、前記シリカ粒子以外の増粘剤、界面活性剤、前記シリカ粒子以外の研磨剤、甘味剤、着色剤、香味剤または防腐剤の一つ以上を含む上記[付記22]に記載の歯磨剤組成物。
[付記24]
前記シリカ粒子は、3〜15μmのメジアン粒径を有する上記[付記22]に記載の歯磨剤組成物。
[付記25]
前記シリカ粒子は、3〜10μmのメジアン粒径を有する上記[付記22]に記載の歯磨剤組成物。
[付記26]
前記シリカ粒子は、30〜80cc/100gの吸油量値を有する上記[付記22]に記載の歯磨剤組成物。
[付記27]
前記シリカ粒子は、50〜350m 2 /gのBET表面積を有する上記[付記22]に記載の歯磨剤組成物。
[付記28]
前記組成物は、少なくとも100の放射性象牙質研磨(RDA)値を有する上記[付記22]に記載の歯磨剤組成物。
[付記29]
前記組成物は、少なくとも85の外被清浄比(PCR)値を有する上記[付記22]に記載の歯磨剤組成物。
[付記30]
シリカ粒子を組成物の5〜50重量%の量で含む歯磨剤組成物であって、前記シリカ粒子が3〜15μmのメジアン粒径と、100cc/100g超の吸油量値と、20%装填で少なくとも85の外被清浄比(PCR)値とを有する歯磨剤組成物。
[付記31]
前記組成物は、保湿剤、溶媒、結合剤、治療薬、キレート剤、前記シリカ粒子以外の増粘剤、界面活性剤、前記シリカ粒子以外の研磨剤、甘味剤、着色剤、香味剤、または防腐剤の一つ以上を含む上記[付記30]に記載の歯磨剤組成物。
[付記32]
前記シリカ粒子は、3〜10μmのメジアン粒径を有する上記[付記30]に記載の歯磨剤組成物。
[付記33]
前記シリカ粒子は、30〜80cc/100gの吸油量値を示す上記[付記30]に記載の歯磨剤組成物。
[付記34]
前記シリカ粒子は、50〜350m 2 /gのBET表面積を有する上記[付記30]に記載の歯磨剤組成物。
[付記35]
前記組成物は、少なくとも100の放射性象牙質研磨(RDA)値を示す上記[付記30]に記載の歯磨剤組成物。
Claims (13)
- 最大100cc/100gの吸油量値を有するシリカ粒子であって、該シリカ粒子の少なくとも80%を丸々としたものに丸め、0.9超の球形度(S80)因子および8.0mg損失/100,000回転未満のブラス・アインレーナー摩耗値を有するシリカ粒子。
- 前記シリカ粒子は、3〜15μmのメジアン粒径を有する請求項1に記載のシリカ粒子。
- 前記シリカ粒子は、3〜10μmのメジアン粒径を有する請求項1に記載のシリカ粒子。
- 前記シリカ粒子は、30〜80cc/100gの吸油量値を有する請求項1に記載のシリカ粒子。
- 前記シリカ粒子は、50〜350m2/gのBET表面積を有する請求項1に記載のシリカ粒子。
- シリカ粒子を組成物の5〜50重量%の量で含む歯磨剤組成物であって、前記シリカ粒子が100cc/100gまでの吸油量値と、0.9超の球形度(S80)因子と、8.0mg損失/100,000回転未満のブラス・アインレーナー摩耗値とを有し、シリカ粒子の少なくとも80%が丸々としたものに丸められた歯磨剤組成物。
- 前記組成物は、保湿剤、溶媒、結合剤、治療薬、キレート剤、前記シリカ粒子以外の増粘剤、界面活性剤、前記シリカ粒子以外の研磨剤、甘味剤、着色剤、香味剤または防腐剤の一つ以上を含む請求項6に記載の歯磨剤組成物。
- 前記シリカ粒子は、3〜15μmのメジアン粒径を有する請求項6に記載の歯磨剤組成物。
- 前記シリカ粒子は、3〜10μmのメジアン粒径を有する請求項6に記載の歯磨剤組成物。
- 前記シリカ粒子は、30〜80cc/100gの吸油量値を有する請求項6に記載の歯磨剤組成物。
- 前記シリカ粒子は、50〜350m2/gのBET表面積を有する請求項6に記載の歯磨剤組成物。
- 前記組成物は、少なくとも100の放射性象牙質研磨(RDA)値を有する請求項6に記載の歯磨剤組成物。
- 前記組成物は、少なくとも85の外被清浄比(PCR)値を有する請求項6に記載の歯磨剤組成物。
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