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1. 发明申请

WO2015138143A1 PROCESS FOR PREPARING HIGH % SOLIDS INORGANIC HOLLOW PARTICLE DISPERSIONS USING AN INTERFACIAL MINIEMULSION SOL-GEL REACTION 审中-公开
标题翻译：使用界面微型溶胶凝胶反应制备高％固体无机中空粒子分散体的方法
公开(公告)号：WO2015138143A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017808
申请日：2015-02-26
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LEE, Hau-Nan , BERNARD, Stephanie A.
IPC分类号： C01B33/18 , C09C1/30 , C09D7/12
CPC分类号： C09C1/30 , A61K8/0279 , A61K8/25 , A61K2800/10 , A61K2800/412 , A61K2800/651 , A61Q19/00 , B01J13/16 , C01B33/18 , C01P2002/01 , C01P2004/04 , C01P2004/34 , C01P2004/62 , C01P2004/64 , C09D1/04 , C09D5/022 , C09D7/40 , C09D7/68
摘要： The disclosure provides a process for making an inorganic hollow particle dispersion at a solids concentration of at least 2 wt% solids through interfacial miniemulsion sol-gel reaction comprising: forming an oil-in-water or water-in-oil minemulsion by high energy shearing at least one non-reactive solvent; at least one solvent-based silica precursor; and at least one surfactant; at an energy density of at least 10^6 J/m^3; wherein the concentration of silica precursor is about 2 to about 10 weight (wt) %; in the absence of a catalyst or alcohol cosolvent; and wherein the silica precursor to non-reactive solvent ratio is about 0.1 to about 6; and oil to water or water to oil ratio is about 0.01 to 0.55; and surfactant concentration is about 0.001 wt % to about 5 wt%; and initiating a one-step sol-gel reaction, or to allow the silica precursor to diffuse to the oil/water interface, where it hydrolyzes and condenses to form a silica shell resulting in silica hollow particles having a particle size of less than about 400 nm being formed.
摘要翻译：本公开提供了通过界面微乳液溶胶 - 凝胶反应制备固体浓度为至少2重量％固体的无机中空颗粒分散体的方法，包括：通过高能量剪切形成水包油或油包水微乳液至少一种非反应性溶剂; 至少一种溶剂基二氧化硅前体; 和至少一种表面活性剂; 在至少10 ^ 6J / m 3的能量密度下; 其中二氧化硅前体的浓度为约2至约10重量％; 在没有催化剂或醇助溶剂的情况下; 并且其中所述二氧化硅前体与非反应性溶剂的比率为约0.1至约6; 油与水或水与油的比例约为0.01〜0.55; 表面活性剂浓度为约0.001重量％至约5重量％; 并开始一步溶胶 - 凝胶反应，或允许二氧化硅前体扩散到油/水界面，在那里它水解并冷凝形成二氧化硅壳，导致粒度小于约400的二氧化硅中空颗粒 nm。

2. 发明申请

WO2015138163A1 PROCESS FOR PREPARING FLUORINATED POLYMERIC HOLLOW NANOSPHERES 审中-公开
标题翻译：制备氟化中性纳米粒子的方法
公开(公告)号：WO2015138163A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017915
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LEE, Hau-Nan , RAGHAVANPILLAI, Anilkumar , BERNARD, Stephanie A.
IPC分类号： C08F2/22 , C08F2/44 , B82Y30/00
CPC分类号： C08F2/22 , A61K8/0279 , A61K8/8117 , A61K2800/10 , A61K2800/412 , A61Q19/00 , B01J13/14 , B82Y40/00 , C08F2/44
摘要： The disclosure provides a process for preparing a fluorinated polymeric hollow nanosphere comprising: providing a mixture comprising water, at least one non-reactive solvent, at least one acrylic or styrenic monomer; at least at least one fluorinated acrylic monomer; an initiator; and at least one surfactant; shearing the components of the mixture with high shear energy at an energy density of at least 10^6 J/m^3 to form a mini-emulsion; and heating to at least about 50C to form, in one step, a fluorinated polymeric hollow nanosphere.
摘要翻译：本公开提供了制备氟化聚合物中空纳米球的方法，其包括：提供包含水，至少一种非反应性溶剂，至少一种丙烯酸或苯乙烯单体的混合物; 至少一种氟化丙烯酸单体; 发起者和至少一种表面活性剂; 以至少10 6 J / m 3的能量密度以高剪切能剪切混合物的组分以形成微乳液; 并加热至至少约50℃，以一步形成氟化聚合物中空纳米球。

3. 发明申请

WO2015138154A1 PROCESS FOR PREPARING SILICA/POLYMER HYBRID HOLLOW NANOSPHERES USING WATER-BASED SILICA PRECURSORS 审中-公开
标题翻译：使用水基二氧化硅前驱体制备二氧化硅/聚合物混合中空纳米微粒的方法
公开(公告)号：WO2015138154A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017899
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LEE, Hau-Nan , BERNARD, Stephanie A
IPC分类号： C08F2/22 , C08F2/44 , B82Y30/00
CPC分类号： C08F2/22 , A61K8/0279 , A61K8/25 , A61K8/8117 , A61K8/8152 , A61K2800/10 , A61Q19/00 , B01J13/14 , B82Y40/00 , C08F2/44 , C08F220/14 , C08F212/08 , C08F2222/1013
摘要： The disclosure provides a process for preparing a silica/polymeric hybrid hollow nanosphere comprising: providing a mixture comprising water, at least one non-reactive solvent; at least one acrylic or styrenic monomer; an initiator; and at least one surfactant; shearing the components of the above mixture with high shear energy at an energy density of at least 10^6 J/m^3 to form a mini-emulsion; heating to at least about 50 °C to initiate the polymerization reaction; and at the same time, feeding at least one water-based silica precursor solution to emulsion; and adjusting the pH to about 4 to 10 so that the water-based silica precursor hydrolyzes and condenses to form a silica shell at the oil/water interface resulting in silica/polymeric hybrid hollow nanospheres. Steps (c) and (d) in this process may occur simultaneously.
摘要翻译：本公开提供了一种制备二氧化硅/聚合物混合中空纳米球的方法，包括：提供包含水，至少一种非反应性溶剂的混合物; 至少一种丙烯酸或苯乙烯单体; 发起者和至少一种表面活性剂; 以至少10 ^ 6J / m 3的能量密度以高剪切能剪切上述混合物的组分以形成微乳液; 加热至至少约50℃以引发聚合反应; 同时将至少一种水性二氧化硅前体溶液加入乳液中; 并将pH调节至约4至10，使得水基二氧化硅前体在油/水界面处水解并冷凝以形成二氧化硅壳，得到二氧化硅/聚合混合中空纳米球。此过程中的步骤（c）和（d）可能同时发生。

4. 发明申请

WO2015138156A1 PROCESS FOR PREPARING FLUORINATED, INORGANIC HOLLOW NANOSPHERES USING WATER-BASED SILICA PRECURSORS 审中-公开
标题翻译：使用水基二氧化硅前体制备无色无色中空纳米微球的方法
公开(公告)号：WO2015138156A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017903
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LEE, Hau-Nan , LASIO, Jelena , RAGHAVANPILLAI, Anilkumar , BERNARD, Stephanie A
IPC分类号： C09C1/30
CPC分类号： C09C1/3081 , A61K8/0279 , A61K8/25 , A61K9/501 , A61K9/5089 , A61K2800/10 , A61Q19/00 , B01J13/16 , C01P2004/04 , C01P2004/34 , C01P2004/62 , C01P2004/64
摘要： The disclosure provides a process for preparing a fluorinated silica hollow nanosphere comprising: providing a mixture comprising water, at least one non-reactive solvent, at least one fluorosilane, at least one water based silica precursor solution, such as sodium silicate, potassium silicate, ammonium silicate or pre-formed silicic acid, and at least one surfactant; shearing the components of the mixture with high shear energy at an energy density of at least 10^6 J/m^3 to form a mini-emulsion; initiating a one-step sol-gel reaction by adjusting the pH to about 4 to 10 and then initiating a one-step sol-gel forming fluorinated hollow silica nanospheres having a particle size of less than about 400nm.
摘要翻译：本公开提供了一种制备氟化二氧化硅中空纳米球的方法，其包括：提供包含水，至少一种非反应性溶剂，至少一种氟硅烷，至少一种水基二氧化硅前体溶液如硅酸钠，硅酸钾，硅酸铵或预形成的硅酸，和至少一种表面活性剂; 以至少10 6 J / m 3的能量密度以高剪切能剪切混合物的组分以形成微乳液; 通过将pH调节至约4至10，然后引发一步溶胶 - 凝胶形成具有小于约400nm的粒度的氟化中空二氧化硅纳米球，开始一步溶胶 - 凝胶反应。

5. 发明申请

WO2015138155A1 PROCESS FOR PREPARING INORGANIC HOLLOW PARTICLE DISPERSIONS USING AN INTERFACIAL MINIEMULSION SOL-GEL REACTION AND A WATER-BASED PRECURSOR 审中-公开
标题翻译：使用界面微型溶胶凝胶反应和基于水的前驱体制备无机中空粒子分散体的方法
公开(公告)号：WO2015138155A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017901
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LEE, Hau-Nan , BERNARD, Stephanie A
IPC分类号： C01B33/18 , C09C1/30
CPC分类号： C09C1/30 , A61K8/0279 , A61K8/25 , A61K9/501 , A61K9/5089 , A61K2800/10 , A61Q19/00 , B01J13/16 , C01B33/18 , C01P2002/01 , C01P2004/04 , C01P2004/34 , C01P2004/62 , C01P2004/64 , C01P2004/90
摘要： The disclosure provides a process for making an inorganic hollow particle dispersion using water based precursors through an interfacial miniemulsion sol-gel reaction comprising: a) forming an oil-in-water or water-in-oil minemulsion by high energy shearing water, at least one non-reactive solvent; and at least one surfactant; at an energy density of at least 10^6 J/m^3; wherein the oil to water or water to oil ratio is about 0.01 to about 0.55; and surfactant concentration is about 0.001 wt % to about 5 wt %, based on the total weight of the dispersion; b) adjusting the pH of the emulsion; c) feeding at least one water based silica precursor solution to emulsion at constant feeding rate over several hours wherein the concentration of silica precursor is about 0.005 wt% to about 5 wt%, based on the total weight of the dispersion; while maintaining the pH of the solution at above about 6 or below about 2; d) holding solution at room temperature, with optional stirring to allow the silica precursor to diffuse to the oil/water interface; and e) initiating a one-step sol-gel reaction by adjusting the pH to about 4 to about 10, whereby the water based silica precursor hydrolyzes and condenses to form a silica shell at the oil/water interface resulting in silica hollow particles having a particle size of less than about 400 nm.
摘要翻译：本公开提供了一种通过界面微乳液溶胶 - 凝胶反应制备使用水基前体的无机中空颗粒分散体的方法，包括：a）通过高能量剪切水形成水包油或油包水微乳液，至少一种非反应性溶剂; 和至少一种表面活性剂; 在至少10 ^ 6J / m 3的能量密度下; 其中油与水或水与油的比例为约0.01至约0.55; 并且基于分散体的总重量，表面活性剂浓度为约0.001重量％至约5重量％; b）调节乳液的pH值; c）在几小时内以恒定的进料速率将至少一种水基二氧化硅前体溶液进料至乳液，其中基于分散体的总重量，二氧化硅前体的浓度为约0.005重量％至约5重量％; 同时将溶液的pH保持在约6或更低约2左右; d）在室温下保持溶液，任选搅拌，使二氧化硅前体扩散到油/水界面; 和e）通过将pH调节至约4至约10，引发一步溶胶 - 凝胶反应，由此水基二氧化硅前体在油/水界面处水解并冷凝以形成二氧化硅壳，从而产生二氧化硅中空颗粒，其具有粒度小于约400nm。

6. 发明申请

WO2015138164A1 PROCESS FOR PREPARING SURFACE FUNCTIONALIZED POLYMERIC AND POLYMERIC/SILICA HYBRID HOLLOW NANOSPHERES 审中-公开
标题翻译：表面官能化聚合物和聚合物/二氧化硅混合中空纳米微粒的制备方法
公开(公告)号：WO2015138164A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017916
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LEE, Hau-Nan , BERNARD, Stephanie A. , LASIO, Jelena , DUNCAN, Andrew Jay
IPC分类号： C08F2/22 , C08F2/44 , B82Y30/00
CPC分类号： C08F2/22 , A61K8/0279 , A61K8/25 , A61K8/8117 , A61K8/8152 , A61K2800/10 , A61K2800/413 , A61K2800/614 , A61Q19/00 , B01J13/14 , B82Y40/00 , C08F2/44
摘要： The disclosure provides a process for preparing a surface functionalized polymeric or polymeric/silica hybrid hollow nanospheres comprising: providing a mixture comprising water, at least one non-reactive solvent, at least one acrylic or styrenic monomer; at least one functionalized acrylic or styrenic monomer; an initiator; at least one surfactant; and, optionally, a polymerizable silane if the polymeric/silica hybrid hollow particles are desired; and shearing the components of the mixture with high shear energy at an energy density of at least 10^6 J/m^3 to form a mini-emulsion; and heating to at least about 50°C, more typically about 50°C to about 90°C; and still more typically about 60°C to about 80°C to form, in one step, a surface functionalized polymeric or polymeric/silica hybrid hollow nanosphere.
摘要翻译：本公开提供了制备表面官能化聚合物或聚合物/二氧化硅混合中空纳米球的方法，其包括：提供包含水，至少一种非反应性溶剂，至少一种丙烯酸或苯乙烯单体的混合物; 至少一种官能化丙烯酸或苯乙烯单体; 发起者至少一种表面活性剂; 如果需要聚合物/二氧化硅混合中空颗粒，可选地包含可聚合硅烷; 并以至少10 6 J / m 3的能量密度以高剪切能剪切混合物的组分以形成微乳液; 并加热至至少约50℃，更典型地约50℃至约90℃; 并且还更典型地约60℃至约80℃，以在一个步骤中形成表面官能化的聚合物或聚合物/二氧化硅混合中空纳米球。

7. 发明申请

WO2015138160A1 FUNCTIONALIZED HOLLOW SILICA PARTICLES WITH LOW POROSITY USING WATER-BASED SILICA PRECURSORS 审中-公开
标题翻译：功能化的中空二氧化硅颗粒，使用水基二氧化硅前体具有低孔隙度
公开(公告)号：WO2015138160A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017909
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LASIO, Jelena , LEE, Hau-Nan , RAGHAVANPILLAI, Anilkumar , WHIPPLE, Devin T. , CATIVO, Ma Helen
IPC分类号： C09C1/30 , C01B33/12 , C01B33/149 , C08F2/10 , C08F8/50
CPC分类号： C09C1/3054 , B01J13/18 , B01J13/20 , B01J13/203 , B01J13/22 , C01B33/12 , C01B33/149 , C01B33/18 , C01P2004/04 , C01P2004/34 , C01P2004/61 , C01P2004/62 , C01P2004/64 , C08F2/10 , C08F8/50 , C08F220/14 , C08F220/34 , C08F2222/1013 , C08F230/08
摘要： The disclosure provides a functionalized hollow silica particle comprising: a core/shell silica particle comprising a template core particle and a silica treatment, wherein the core/shell silica particle has an outer surface; and wherein the silica treatment is prepared using a water-based silica precursor; a functionalized surface on the core/shell silica particle, wherein the functionalized surface is prepared using sulfonic acid, phosphonic esters, carboxylic acid, amines, epoxides, or boronic acids, and wherein the template core particle is removed before or after functionation. These inorganic hollow particles are useful as hiding or opacifying agents in coating and molding compositions. They are also useful as photonic band gap or thermal insulation materials.
摘要翻译：本发明提供了一种功能化中空二氧化硅颗粒，其包括：核/壳二氧化硅颗粒，其包含模板核心颗粒和二氧化硅处理，其中所述核/壳二氧化硅颗粒具有外表面; 并且其中所述二氧化硅处理是使用水基二氧化硅前体制备的; 核/壳二氧化硅颗粒上的功能化表面，其中官能化表面使用磺酸，膦酸酯，羧酸，胺，环氧化物或硼酸制备，并且其中在功能化之前或之后除去模板核心颗粒。这些无机中空颗粒可用作涂料和模塑组合物中的遮盖剂或不透明剂。它们也可用作光子带隙或保温材料。

8. 发明申请

WO2015138153A1 PROCESS FOR PREPARING SILICA/POLYMER HYBRID HOLLOW NANOSPHERES THROUGH INTERFACIAL POLYMERIZATION IN INVERSE MINIEMULSIONS 审中-公开
标题翻译：通过反相微观结构中的界面聚合制备二氧化硅/聚合物混合中空纳米微粒的方法
公开(公告)号：WO2015138153A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017898
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LEE, Hau-Nan , BERNARD, Stephanie, A
IPC分类号： C09C1/30 , C01B33/12 , B01J37/00 , C01B37/02 , C08F2/22 , C08F2/24 , C08F2/26 , C08F2/28 , C08F2/30 , C08F2/44
CPC分类号： C09C1/3072 , C01B37/02 , C01P2004/34 , C01P2004/62 , C08F2/22 , C08F2/44 , C08F220/14 , C08F2222/1013 , C08F212/08
摘要： The disclosure provides a process for preparing a silica/polymeric hybrid hollow nanosphere comprising: providing a mixture comprising water, at least one non-reactive solvent; at least one acrylic or styrenic monomer; at least one solvent based silica precursor or a polymerizable silane or combinations thereof; an initiator; and at least one surfactant; shearing the components of the mixture with high shear energy at an energy density of at least 10^6 J/m^3 to form a mini-emulsion; and heating to at least about 50° C to form, in one step, a silica/polymeric hybrid hollow nanosphere.
摘要翻译：本公开提供了一种制备二氧化硅/聚合物混合中空纳米球的方法，包括：提供包含水，至少一种非反应性溶剂的混合物; 至少一种丙烯酸或苯乙烯类单体; 至少一种溶剂基二氧化硅前体或可聚合硅烷或其组合; 发起者和至少一种表面活性剂; 以至少10 6 J / m 3的能量密度以高剪切能剪切混合物的组分以形成微乳液; 并加热至至少约50℃，在一个步骤中形成二氧化硅/聚合混合中空纳米球。

9. 发明申请

WO2015138117A1 COATING COMPOSITIONS COMPRISING HOLLOW SILICA PARTICLES WITH LOW POROSITY 审中-公开
标题翻译：包含具有低孔隙度的中性二氧化硅颗粒的涂料组合物
公开(公告)号：WO2015138117A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017323
申请日：2015-02-24
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： BARNEY, Nathaniel A , CROWTHER JR, John A , ROSEN, Brad M , LASIO, Jelena , LEE, Hau-Nan , DUNCAN, Andrew Jay
IPC分类号： B01J13/14 , C09D7/12 , C09C1/00 , C09C1/30 , C09C1/36 , C23C18/12
CPC分类号： C09C1/30 , B01J13/18 , B01J13/203 , C01P2004/34 , C01P2004/62 , C01P2004/64 , C01P2004/84 , C01P2006/14 , C01P2006/60 , C09C1/0084 , C09C1/3045 , C09C1/3063 , C09C1/36 , C09C1/3607 , C09D5/00 , C09D7/62 , C23C18/1212 , C23C18/122 , C23C18/1229 , C23C18/1233 , C23C18/1245
摘要： The disclosure provides a coating composition having improved opacity comprising a titanium dioxide (TiO 2 ) particle chemically attached to a hollow particle, wherein the hollow particle's size has a volume ratio when compared to the titanium dioxide particle of between 0.008 and 8. These coating compositions comprise inorganic hollow particles which are useful as hiding or opacifying agents.
摘要翻译：本公开提供了一种涂料组合物，其具有改善的不透明度，其包含与中空颗粒化学连接的二氧化钛（TiO 2）颗粒，其中当与二氧化钛颗粒在0.008和8之间时，中空颗粒的尺寸具有体积比。这些涂料组合物包含可用作隐藏或遮光剂的无机中空颗粒。

10. 发明申请

WO2015138159A1 PROCESS FOR PREPARING FUNCTIONALIZED HOLLOW SILICA PARTICLES HAVING LOW POROSITY USING WATER-BASED SILICA PRECURSORS 审中-公开
标题翻译：使用水基二氧化硅前驱体制备具有低孔隙率的功能性中空二氧化硅颗粒的方法
公开(公告)号：WO2015138159A1
公开(公告)日：2015-09-17
申请号：PCT/US2015/017907
申请日：2015-02-27
申请人： E I DU PONT DE NEMOURS AND COMPANY
发明人： LASIO, Jelena , LEE, Hau-Nan , RAGHAVANPILLAI, Anilkumar , CATIVO, Ma Helen
IPC分类号： C09C1/30 , C01B33/12 , C01B33/149 , C08F2/10 , C08F8/50
CPC分类号： C09C1/3054 , C01B33/12 , C01B33/149 , C01B33/18 , C01P2004/34 , C01P2004/62 , C01P2004/64 , C08F2/22 , C08F220/14 , C08F265/04 , C09C1/3063 , C09C1/3081 , C08F230/08 , C08F220/34 , C08F2230/085 , C08F2222/1013
摘要： The disclosure provides a process for preparing the functionalized hollow silica particles comprises: providing a core-shell silica particle comprising a template core particle and a silica treatment, wherein the core-shell silica particle has an outer surface; and wherein the silica treatment is prepared using a water-based silica precursor; creating a functionalized surface on the core-shell silica particle, wherein the functionalized surface is prepared using sulfonic acid, phosphonic esters, carboxylic acid, amines, epoxides, or boronic acids, and removing the template core particle to form a functionalized hollow silica particle. These inorganic hollow particles are useful as hiding or opacifying agents in coating and molding compositions. They are also useful as photonic band gap or thermal insulation materials.
摘要翻译：本发明提供了制备官能化中空二氧化硅颗粒的方法，包括：提供包含模板核心颗粒和二氧化硅处理的核 - 壳二氧化硅颗粒，其中核 - 壳二氧化硅颗粒具有外表面; 并且其中所述二氧化硅处理是使用水基二氧化硅前体制备的; 在核 - 壳二氧化硅颗粒上形成功能化表面，其中功能化表面使用磺酸，膦酸酯，羧酸，胺，环氧化物或硼酸制备，并除去模板核心颗粒以形成官能化的中空二氧化硅颗粒。这些无机中空颗粒可用作涂料和模塑组合物中的隐藏剂或不透明剂。它们也可用作光子带隙或保温材料。

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