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公开(公告)号：US06184408B2
公开(公告)日：2001-02-06
申请号：US09299863
申请日：1999-04-28
申请人： Gary Thomas Burns , Qin Deng , James Richard Hahn , Thomas G. Krivak , Timothy A. Okel , Clifford Carlton Reese
发明人： Gary Thomas Burns , Qin Deng , James Richard Hahn , Thomas G. Krivak , Timothy A. Okel , Clifford Carlton Reese
IPC分类号： C07F708
CPC分类号： C09C1/3081 , C01B33/193 , C01P2006/12 , C01P2006/90
摘要： A method for the preparation of hydrophobic precipitated silica. The method comprises contacting an aqueous suspension of a hydrophilic precipitated silica with (1) a catalytic amount of an acid and (2) an organosilicon compound in the presence of (3) a water-miscible organic solvent in an amount sufficient to facilitate reaction of the hydrophilic precipitated silica with the organosilicon compound to form a hydrophobic precipitated silica.
摘要翻译： 疏水性沉淀二氧化硅的制备方法。 该方法包括在（3）水混溶性有机溶剂存在下使亲水沉淀二氧化硅的水性悬浮液与（1）催化量的酸和（2）有机硅化合物接触，其量足以促进 亲水沉淀二氧化硅与有机硅化合物形成疏水性沉淀二氧化硅。
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2.发明授权Method for making hydrophobic organosilicate-modified silica gels under neutral conditions 失效在中性条件下制备疏水性有机硅酸酯改性硅胶的方法
公开(公告)号：US5789495A
公开(公告)日：1998-08-04
申请号：US806011
申请日：1997-02-24
IPC分类号： C01B33/159 , C01B33/16 , C09C1/30 , C09C3/12 , C08F283/00
CPC分类号： C01B33/16
摘要： The present invention is hydrophobic organosilicate-modified silica gels and a method for their preparation under neutral conditions. The method comprises two steps, where in the first step the pH of an organosilicate-modified silica hydrosol is adjusted with a base to within a range of about pH 3 to pH 7 to facilitate formation of an organosilicate-modified silica hydrogel. In the second step the organosilicate-modified silica hydrogel is contacted with an organosilicon compound in the presence of a catalytic amount of a strong acid to effect hydrophobing of the organosilicate-modified silica hydrogel to form a hydrophobic organosilicate-modified silica gel having a surface area within a range of about 100 m.sup.2 /g to 850 m.sup.2 /g in the dry state. In a preferred process the hydrophobic organosilicate-modified silica hydrogel is contacted with a sufficient quantity of a water-immiscible organic solvent to convert the hydrophobic organosilicate-modified silica hydrogel into a hydrophobic organosilicate-modified silica organogel. A water soluble compound of cerium or iron may be added in the second step to improve the heat stability of the hydrophobic organosilicate-modified silica gel.
摘要翻译： 本发明是疏水性有机硅酸酯改性二氧化硅凝胶及其在中性条件下制备的方法。 该方法包括两个步骤，其中在第一步中，将有机硅酸酯改性的二氧化硅水溶胶的pH用碱调节至约pH 3至pH 7的范围内，以促进形成有机硅酸酯改性的二氧化硅水凝胶。 在第二步中，有机硅酸酯改性的二氧化硅水凝胶在催化量的强酸存在下与有机硅化合物接触，以实现有机硅酸酯改性的二氧化硅水凝胶的疏水化，从而形成具有表面积的疏水性有机硅酸酯改性硅胶 在干燥状态下在约100m 2 / g至850m 2 / g的范围内。 在优选的方法中，将疏水性有机硅酸酯改性的二氧化硅水凝胶与足够量的与水不混溶的有机溶剂接触以将疏水性有机硅酸酯改性的二氧化硅水凝胶转化成疏水性有机硅酸酯改性的二氧化硅有机凝胶。 可以在第二步中加入铈或铁的水溶性化合物，以提高疏水性有机硅酸酯改性硅胶的热稳定性。
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公开(公告)号：US6107351A
公开(公告)日：2000-08-22
申请号：US28038
申请日：1998-02-23
CPC分类号： B82Y30/00 , C01B33/16 , C09C1/3081 , C01P2004/64 , C01P2006/12 , C01P2006/14 , C01P2006/16 , C01P2006/22 , C01P2006/80 , C01P2006/90 , Y10T428/2995
摘要： The present invention is neutral-aged hydrophobic silica gels having a reduced surface area and a method for their preparation. The method comprises three steps, where in the first step a mixture comprising a silica hydrosol and colloidal silica is contacted with a strong mineral acid at a pH less than about 1 to form a silica hydrogel having incorporated therein colloidal silica. In the second step the silica hydrogel is aged at a pH within a range of about pH 3.5 to pH 8. In the third step the silica hydrogel is contacted with an organosilicon compound in the presence of a catalytic amount of a strong acid to effect hydrophobing of the silica hydrogel to form a hydrophobic silica hydrogel having a surface area within a range of about 100 m.sup.2 /g to 450 m.sup.2 /g in the dry state. In a preferred method the hydrophobic silica hydrogel and is further contacted with a sufficient quantity of a water-immiscible organic solvent to convert the hydrophobic silica hydrogel into a hydrophobic silica organogel.
摘要翻译： 本发明是具有减小的表面积的中性疏水性硅胶，及其制备方法。 该方法包括三个步骤，其中在第一步骤中，将包含二氧化硅水溶胶和胶体二氧化硅的混合物与pH值小于约1的强无机酸接触以形成掺入胶体二氧化硅的二氧化硅水凝胶。 在第二步中，将二氧化硅水凝胶在约3.5至约8的pH范围内老化。在第三步中，在催化量的强酸存在下，使二氧化硅水凝胶与有机硅化合物接触以进行疏水 的二氧化硅水凝胶以形成在干燥状态下表面积在约100m 2 / g至450m 2 / g范围内的疏水性二氧化硅水凝胶。 在优选的方法中，疏水性二氧化硅水凝胶进一步与足够量的与水不混溶的有机溶剂接触以将疏水性二氧化硅水凝胶转化成疏水性二氧化硅有机凝胶。
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4.发明授权Process for making hydrophobic silica with reduced surface area under neutral conditions 失效在中性条件下制备表面积减小的疏水性二氧化硅的方法
公开(公告)号：US5942590A
公开(公告)日：1999-08-24
申请号：US22282
申请日：1998-02-11
IPC分类号： C01B33/159 , C01B33/16 , C09C1/30 , C08G77/00
CPC分类号： B82Y30/00 , C01B33/16 , C09C1/3081 , C09C1/309 , C01P2004/51 , C01P2004/64 , C01P2006/12 , C01P2006/90
摘要： The present invention is hydrophobic silica gels having a reduced surface area and a method for their preparation under neutral conditions. The method comprises two steps, where in the first step the pH of a mixture comprising a silica hydrosol and colloidal silica is adjusted with a base to within a range of pH 3 to pH 6 to facilitate formation of a silica hydrogel having incorporated therein colloidal silica. In the second step the silica hydrogel is contacted with an organosilicon compound in the presence of a catalytic amount of a strong acid to effect hydrophobing of the silica hydrogel to form a hydrophobic silica gel having a surface area within a range of about 100 m.sup.2 /g to 450 m.sup.2 /g in the dry state. In a preferred process the hydrophobic silica gel is contacted with a sufficient quantity of a water-immiscible organic solvent to convert the hydrophobic silica hydrogel into a hydrophobic silica organogel. A water soluble compound of cerium or iron may be added during conduct of the second step to improve heat stability of the hydrophobic silica gel.
摘要翻译： 本发明是具有减小的表面积的疏水性硅胶和其在中性条件下制备的方法。 该方法包括两个步骤，其中在第一步骤中，将包含二氧化硅水溶胶和胶体二氧化硅的混合物的pH调节至碱在pH 3至pH 6的范围内，以促进形成掺入胶体二氧化硅的二氧化硅水凝胶 。 在第二步骤中，二氧化硅水凝胶在催化量的强酸存在下与有机硅化合物接触，以实现二氧化硅水凝胶的疏水化，从而形成表面积在约100m 2 / g范围内的疏水性硅胶 在干燥状态下为450m2 / g。 在优选的方法中，将疏水性硅胶与足够量的与水不混溶的有机溶剂接触以将疏水性二氧化硅水凝胶转化成疏水性二氧化硅有机凝胶。 在第二步进行时可以加入铈或铁的水溶性化合物，以提高疏水硅胶的热稳定性。
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公开(公告)号：US5807501A
公开(公告)日：1998-09-15
申请号：US801410
申请日：1997-02-20
IPC分类号： C01B33/159 , C01B33/16 , C09C1/30 , B01J13/00 , C04B14/04
CPC分类号： C01B33/16 , C09C1/3081 , C01P2004/61 , C01P2006/12 , C01P2006/14 , C01P2006/16 , C01P2006/22 , C01P2006/60 , C01P2006/90 , Y10T428/2995
摘要： The present invention is neutral-aged hydrophobic organosilicate-modified silica gels and a method for their preparation. The method comprises three steps, where in the first step an organosilicate-modified silica hydrosol is contacted with a strong mineral acid at a pH less than about 1 to form an organosilicate-modified silica hydrogel. In the second step the organosilicate-modified silica hydrogel is aged at a pH within a range of about pH 3.5 to pH 8. In the third step the neutral-aged organosilicate-modified silica hydrogel is contacted with an organosilicon compound in the presence of a catalytic amount of a strong acid to effect hydrophobing of the organosilicate-modified silica hydrogel to form a hydrophobic organosilicate-modified silica hydrogel having a surface area within a range of about 100 m.sup.2 /g to 750 m.sup.2 /g in the dry state. In a preferred process the hydrophobic organosilicate-modified silica hydrogel is contacted with a sufficient quantity of a water-immiscible organic solvent to convert the hydrophobic organosilicate-modified silica hydrogel into a hydrophobic organosilicate-modified silica organogel.
摘要翻译： 本发明是中性老化的疏水性有机硅酸酯改性硅胶及其制备方法。 该方法包括三个步骤，其中在第一步中，将有机硅酸酯改性的二氧化硅水溶胶与pH值小于约1的强无机酸接触以形成有机硅酸酯改性的二氧化硅水凝胶。 在第二步中，将有机硅酸酯改性的二氧化硅水凝胶在pH值约为3.5至pH8的范围内老化。在第三步中，将中性有机硅酸酯改性的二氧化硅水凝胶与有机硅化合物在 催化量的强酸以实现有机硅酸酯改性二氧化硅水凝胶的疏水化，从而形成疏水性有机硅酸酯改性二氧化硅水凝胶，其在干燥状态下的表面积为约100m 2 / g至750m 2 / g。 在优选的方法中，将疏水性有机硅酸酯改性的二氧化硅水凝胶与足够量的与水不混溶的有机溶剂接触以将疏水性有机硅酸酯改性的二氧化硅水凝胶转化成疏水性有机硅酸酯改性的二氧化硅有机凝胶。
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公开(公告)号：US5708069A
公开(公告)日：1998-01-13
申请号：US805398
申请日：1997-02-24
IPC分类号： C01B33/159 , C08K9/06 , C09C1/28 , C09C3/12 , C08K3/10
CPC分类号： C08K9/06 , Y10T428/2962 , Y10T428/2995
摘要： The present invention is hydrophobic silica gels and a method for their preparation under neutral conditions. The method comprises two steps, where in the first step the pH of a silica hydrosol is adjusted with a base to within a range of about pH 3 to pH 7 to facilitate formation of a silica hydrogel. In the second step the silica hydrogel is contacted with an organosilicon compound in the presence of a catalytic amount of a strong acid to effect hydrophobing of the silica hydrogel. In a preferred method, in a third step the hydrophobic silica gel is contacted with a sufficient quantity of a water-immiscible organic solvent to convert the hydrophobic silica hydrogel into a hydrophobic silica organogel.
摘要翻译： 本发明是疏水性硅胶及其在中性条件下制备的方法。 该方法包括两个步骤，其中在第一步骤中，将二氧化硅水溶胶的pH用碱调节至约pH 3至pH 7的范围内以促进二氧化硅水凝胶的形成。 在第二步中，二氧化硅水凝胶在催化量的强酸存在下与有机硅化合物接触，以实现二氧化硅水凝胶的疏水。 在优选的方法中，在第三步骤中，将疏水性硅胶与足够量的与水不混溶的有机溶剂接触以将疏水性二氧化硅水凝胶转化成疏水性二氧化硅有机凝胶。
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7.发明授权Chemically modified silica fillers, process for producing, and silicone compositions containing same 有权化学改性的二氧化硅填料，制备方法和含有它们的硅氧烷组合物公开(公告)号：US06384125B1
公开(公告)日：2002-05-07
申请号：US09637953
申请日：2000-08-11
申请人： Debora Frances Bergstrom , Lisa Marie Boswell , Mark David Fisher , James Richard Hahn , Timothy A. Okel , Clifford Carlton Reese
发明人： Debora Frances Bergstrom , Lisa Marie Boswell , Mark David Fisher , James Richard Hahn , Timothy A. Okel , Clifford Carlton Reese
IPC分类号： C08K334
CPC分类号： B82Y30/00 , B60C1/00 , C01P2004/64 , C01P2006/12 , C08K9/04 , C08K9/06 , C09C1/3027 , C09C1/3054 , C09C1/3063 , C09C1/3081 , C09C1/309 , C09C3/006 , C09C3/08 , C09C3/12 , C08L21/00
摘要： This invention is a process for making modified silica filler comprising the steps of: (A) contacting an acidic aqueous suspension of precipitated or colloidal silica, optionally in the presence of a surfactant and/or a water-miscible solvent, with a combination of (a) a functionalizing coupling agent, and (b) an organometallic hydrophobing compound in a weight ratio of (a) to (b) of at least 0.001 to 1 to form an acidic aqueous suspension of chemically treated silica filler having a pH of 2.0 or less (B) treating the acidic aqueous suspension of the chemically treated filler with an acid-neutralizing agent to increase the pH of the suspension to a range of from greater than 2.0 to 10, and (C) recovering the chemically treated filler. This invention is also modified silica filler that has a pH of from about 5.0 to 10.0, where the silica filler is made by the method of this invention. This invention is also a curable silicone elastomer composition comprising a polyorganosiloxane, the modified silica filler produced by the method of this invention, and a means of curing the polyorganosiloxane into an elastomer.
摘要翻译： 本发明是一种制备改性二氧化硅填料的方法，其包括以下步骤：（A）任选在表面活性剂和/或水混溶性溶剂存在下，使沉淀或胶体二氧化硅的酸性水性悬浮液与（ a）官能化偶联剂，和（b）重量比为（a）至（b）的有机金属疏水化合物为至少0.001至1，以形成pH为2.0的化学处理二氧化硅填料的酸性水性悬浮液，或 （B）用酸中和剂处理化学处理的填料的酸性水性悬浮液以将悬浮液的pH值提高到大于2.0-10的范围，和（C）回收化学处理的填料。本发明 也是pH为约5.0至10.0的改性二氧化硅填料，其中二氧化硅填料通过本发明的方法制备。 本发明还是一种可固化的硅氧烷弹性体组合物，其包含聚有机硅氧烷，通过本发明的方法制备的改性二氧化硅填料，以及将聚有机硅氧烷固化成弹性体的方法。
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公开(公告)号：US5750610A
公开(公告)日：1998-05-12
申请号：US805102
申请日：1997-02-24
CPC分类号： C08K9/06
摘要： The present invention is hydrophobic organosilicate-modified silica gels and a method for their preparation. The method comprises two steps, where in the first step an organosilicate-modified silica hydrosol is heat treated in the presence of a strong mineral acid at a pH less than about pH 1 to form an organosilicate-modified silica hydrogel. In the second step the organosilicate-modified silica hydrogel is contacted with an organosilicon compound in the presence of a catalytic amount of a strong acid to effect hydrophobing of the organosilicate-modified silica hydrogel thereby forming a hydrophobic organosilicate-modified silica hydrogel having a surface area within a range of about 100 m.sup.2 /g to 750 m.sup.2 /g as measured in the dry state. In a preferred method the hydrophobic organosilicate-modified silica gel is contacted with a sufficient quantity of a water-immiscible organic solvent to convert the hydrophobic organosilicate-modified silica hydrogel into a hydrophobic organosilicate-modified silica organogel.
摘要翻译： 本发明是疏水性有机硅酸酯改性硅胶及其制备方法。 该方法包括两个步骤，其中在第一步中，在pH小于约pH 1的强无机酸存在下，将有机硅酸酯改性的二氧化硅水溶胶进行热处理，形成有机硅酸酯改性的二氧化硅水凝胶。 在第二步中，有机硅酸酯改性的二氧化硅水凝胶在催化量的强酸存在下与有机硅化合物接触，以进行有机硅酸酯改性的二氧化硅水凝胶的疏水，从而形成具有表面积的疏水性有机硅酸酯改性二氧化硅水凝胶 在干燥状态下测量的约100m 2 / g至750m 2 / g的范围内。 在优选的方法中，将疏水性有机硅酸酯改性的硅胶与足够量的与水不混溶的有机溶剂接触以将疏水性有机硅酸酯改性的二氧化硅水凝胶转化成疏水性有机硅酸酯改性的二氧化硅有机凝胶。
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公开(公告)号：US5789514A
公开(公告)日：1998-08-04
申请号：US806016
申请日：1997-02-24
CPC分类号： C01B33/16
摘要： A method for the preparation of hydrophobic silica gels which are useful as reinforcing fillers in rubber compositions. The method comprises two steps, where in the first step a silica hydrosol is contacted with a sufficient concentration of a strong mineral acid at a pH less than about pH 1 to form a silica hydrogel. In the second step the silica hydrogel is contacted with described organosilicon compounds in the presence of a catalytic amount of a strong acid to effect hydrophobing of the silica hydrogel thereby forming a hydrophobic silica gel having a surface area within a range of about 100 m.sup.2 /g to 750 m.sup.2 /g as measured in the dry state. In a preferred method the hydrophobic silica hydrogel is contacted with a sufficient quantity of a water-immiscible organic solvent to convert the hydrophobic silica hydrogel into a hydrophobic silica organogel.
摘要翻译： 疏水性硅胶的制备方法，其用作橡胶组合物中的增强填料。 该方法包括两个步骤，其中在第一步骤中，将二氧化硅水溶胶与足够浓度的强无机酸在pH小于约pH 1下接触以形成二氧化硅水凝胶。 在第二步中，二氧化硅水凝胶在催化量的强酸存在下与所述的有机硅化合物接触，以实现二氧化硅水凝胶的疏水，从而形成表面积在约100m 2 / g范围内的疏水性硅胶 在干燥状态下测量为750m 2 / g。 在优选的方法中，将疏水性二氧化硅水凝胶与足够量的与水不混溶的有机溶剂接触以将疏水性二氧化硅水凝胶转化为疏水性二氧化硅有机凝胶。
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公开(公告)号：US06743509B2
公开(公告)日：2004-06-01
申请号：US10263439
申请日：2002-10-01
申请人： Debora Frances Bergstrom , Gary Thomas Burns , Sarah Bridget Granzo , Csilla Kollar , Clifford Carlton Reese
发明人： Debora Frances Bergstrom , Gary Thomas Burns , Sarah Bridget Granzo , Csilla Kollar , Clifford Carlton Reese
IPC分类号： C08K326
CPC分类号： C09C3/12 , C01P2006/12 , C01P2006/80 , C09C1/021 , Y10T428/2993 , Y10T428/2995
摘要： Treating compositions for application to particles of a filler consist of 5-95 percent by weight of a silicon atom containing hydrophobic-type treating agent, and 5-95 percent by weight of a silicon atom containing functional-type treating agent, based on the weight of the composition. Useful functional-type treating agents include bis(alkoxysilylalkyl)polysulfides and mercaptoorganosilicon compounds. Useful hydrophobic-type treating agents include polyorganohydrogensiloxanes and silanol terminated silicone oligomers. The filler most preferred is precipitated (i.e., synthetic) calcium carbonate.
摘要翻译： 用于施用于填料颗粒的组合物由5-95重量％的含有疏水型处理剂的硅原子组成，和5-95重量％的含硅原子的功能型处理剂，基于重量 的组成。 有用的功能型处理剂包括双（烷氧基甲硅烷基烷基）多硫化物和巯基有机硅化合物。 有用的疏水型处理剂包括聚有机氢硅氧烷和硅烷醇封端的硅氧烷低聚物。 最优选的填料是沉淀的（即合成的）碳酸钙。
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