公开(公告)号：US08563620B2

公开(公告)日：2013-10-22

申请号：US13123350

申请日：2009-10-01

申请人： Mohamed Bouazaoui ,  Bruno Capoen ,  Hicham El-Hamzaoui ,  Laurent Bigot ,  Géraud Bouwmans

发明人： Mohamed Bouazaoui ,  Bruno Capoen ,  Hicham El-Hamzaoui ,  Laurent Bigot ,  Géraud Bouwmans

IPC分类号： C03B19/12 ,  C03C3/06

CPC分类号： C03B19/12 ,  C03B37/016 ,  C03B2201/04 ,  C03B2203/42 ,  C03C1/006 ,  C03C3/06

摘要： The process for the synthesis of a silica monolith comprises the following steps: hydrolysis of a silicon alkoxide in order to form a hydrolysis precursor followed by a condensation of said hydrolysis precursor in the presence of an organic solvent, in the presence of water and of a basic catalyst in order to form oligomeric clusters containing several silicon atoms; dispersion of said oligomeric clusters in a solution in order to form a sol; polymerization of the sol in order to obtain a gel via a first heat treatment, at a temperature below the boiling point of the constituents of the sol; drying of the gel via a second heat treatment; conversion of the gel to a xerogel via a third heat treatment; dehydration and densification of the xerogel until the silica monolith is obtained via a fourth heat treatment.

摘要翻译： 用于合成二氧化硅整料的方法包括以下步骤：水解硅烷醇以形成水解前体，随后在有机溶剂存在下，在水和有机溶剂存在下使所述水解前体缩合 碱性催化剂，以形成含有几个硅原子的低聚簇; 将所述低聚簇分散在溶液中以形成溶胶; 在低于溶胶成分的沸点的温度下通过第一热处理获得凝胶的溶胶的聚合; 通过第二次热处理干燥凝胶; 通过第三次热处理将凝胶转化为干凝胶; 干凝胶的脱水和致密化直到通过第四次热处理获得二氧化硅整料。

公开(公告)号：US20110201714A1

公开(公告)日：2011-08-18

申请号：US13123350

申请日：2009-10-01

申请人： Mohamed Bouazaoui ,  Bruno Capoen ,  Hicham El-Hamzaoui ,  Laurent Bigot ,  Géraud Bouwmans

发明人： Mohamed Bouazaoui ,  Bruno Capoen ,  Hicham El-Hamzaoui ,  Laurent Bigot ,  Géraud Bouwmans

IPC分类号： C08J9/36 ,  C08G77/04

CPC分类号： C03B19/12 ,  C03B37/016 ,  C03B2201/04 ,  C03B2203/42 ,  C03C1/006 ,  C03C3/06

摘要： The present invention relates to a process for the synthesis of a silica monolith according to a process known as a “sol-gel process” that comprises the following steps: hydrolysis of a silicon alkoxide in order to form a hydrolysis precursor followed by a condensation of said hydrolysis precursor in the presence of an organic solvent, in the presence of water and of a basic catalyst in order to form oligomeric clusters containing several silicon atoms; dispersion of said oligomeric clusters in a solution in order to form a sol; polymerization of the sol in order to obtain a gel via a first heat treatment, at a temperature below the boiling point of the constituents of the sol; drying of the gel via a second heat treatment including an exposure of the gel to around 90° C. for at least 24 hours followed by an increase in temperature, under vacuum, between around 90° C. and around 180° C., said temperature increase being between 0.1/min and 5° C./min; conversion of the gel to a xerogel via a third heat treatment, said heat treatment including a hold at a drying temperature between 850 and 1000° C. for at least an hour; dehydration and densification of the xerogel until the silica monolith is obtained via a fourth heat treatment, said fourth heat treatment comprising a hold at a temperature above 1100° C. for at least one hour. The present invention also relates to a silica monolith obtained by the process of the invention, having a concentration of —OH groups of less than 1 ppm. The present invention also discloses the use of the monolith of the invention for producing optical fibres.

摘要翻译： 本发明涉及根据已知为“溶胶 - 凝胶法”的方法合成二氧化硅整料的方法，该方法包括以下步骤：水解硅烷醇以形成水解前体，然后冷凝 所述水解前体在有机溶剂的存在下，在水和碱性催化剂的存在下，以形成含有几个硅原子的低聚簇; 将所述低聚簇分散在溶液中以形成溶胶; 在低于溶胶成分的沸点的温度下通过第一热处理获得凝胶的溶胶的聚合; 通过第二热处理干燥凝胶，包括将凝胶暴露于约90℃至少24小时，然后在真空下在约90℃至约180℃之间升高温度，所述 温度升高在0.1 / min〜5℃/ min之间; 通过第三次热处理将凝胶转化为干凝胶，所述热处理包括在850至1000℃之间的干燥温度下保持至少1小时; 干凝胶的脱水和致密化直到通过第四次热处理获得二氧化硅整料，所述第四热处理包括在高于1100℃的温度下保持至少1小时。 本发明还涉及通过本发明的方法得到的二氧化硅石墨，其浓度小于1ppm。 本发明还公开了本发明的整料用于生产光纤的用途。