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    Process for the production of precipitated silica
    1.
    发明授权
    Process for the production of precipitated silica 失效
    沉淀二氧化硅的生产工艺

    公开(公告)号：US5484581A

    公开(公告)日：1996-01-16

    申请号：US285672

    申请日：1994-08-04

    申请人： Heinz Esch ,  Robert Kuhlmann ,  Mattias Neumueller ,  Karin Otto ,  Ralf Rausch

    发明人： Heinz Esch ,  Robert Kuhlmann ,  Mattias Neumueller ,  Karin Otto ,  Ralf Rausch

    IPC分类号： A61K8/00 ,  A61K8/25 ,  A61Q11/00 ,  C01B33/193 ,  A61K7/16 ,  A61K7/18 ,  C01B33/12 ,  C09K3/14

    CPC分类号： C01B33/193 ,  A61K8/25 ,  A61Q11/00 ,  C01P2004/61 ,  C01P2006/12 ,  C01P2006/22

    摘要： Precipitated silica which has a BET surface area of 10-130 m.sup.2 /g, a CTAB surface area of 10-70 m.sup.2 /g , an average particle diameter of 5-20 .mu.m, a Cu abrasion value in a 10% glycerol dispersion of 4-50 mg and thickening behavior in a CMC solution (20% dispersion) of 300-3500 mPa.multidot.s, is produced by simultaneously adding alkali silicate (weight modulus SiO.sub.2 :alkali oxide=2.5-3.9:1) and a mineral acid to an initial amount of water which has been adjusted to a pH value of 7.0 to 9.9 or 10.0 to 10.7 by the addition of water glass, holding the pH value constant between 7.0 and 9.9 or 10.0 to 10.7 during addition, wherein the initial precipitation temperature is 50.degree.-90.degree. C. and an increase in viscosity occurs after at most 25% of the duration of precipitation, adjusting the pH value to .ltoreq.6, preferably 3.5, once a silica content of greater than 120 g/l or greater than 150 g/l, preferably .gtoreq.160 g/l to 240 g/l, has been reached, separating the solid by filtration, washing, drying and grinding it. The precipitated silica may be used as an abrasive and/or thickening component in toothpastes.

    摘要翻译： BET表面积为10-130m2 / g，CTAB表面积为10-70m2 / g，平均粒径为5-20μm的沉淀二氧化硅，10％甘油分散体中的Cu磨损值 通过同时将碱金属硅酸盐（重量模量SiO 2：碱金属氧化物= 2.5-3.9:1）和无机酸同时加入到初始浓度为300-3500mPax的CMC溶液（20％分散体）中，4-50mg和增稠行为 通过加入水玻璃将pH值调节至pH7.0〜9.9或10.0〜10.7的水，在添加时保持pH值在7.0〜9.9或10.0〜10.7之间，其中初始沉淀温度为50℃ -90℃，并且在沉淀持续时间的至多25％之后发生粘度增加，一旦二氧化硅含量大于120g / l或大于150，则将pH值调节至≤6，优选3.5。 g / l，优选> = = 160g / l至240g / l，通过过滤，洗涤，干燥和研磨分离固体 注意 沉淀二氧化硅可用作牙膏中的研磨剂和/或增稠组分。

    Precipitated silicas
    3.
    发明授权
    Precipitated silicas 失效
    沉淀二氧化硅

    公开(公告)号：US5846506A

    公开(公告)日：1998-12-08

    申请号：US891448

    申请日：1997-07-10

    申请人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    发明人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    IPC分类号： C01B33/193 ,  C01B33/142

    CPC分类号： C01B33/193 ,  C01P2004/50 ,  C01P2004/61 ,  C01P2004/62 ,  C01P2006/12 ,  C01P2006/14 ,  C01P2006/19

    摘要： A precipitated silica with the following physicochemical properties: ______________________________________ BET surface area 35 to 350 m.sup.2 /g BET/CTAB surface area ratio 0.8 to 1.1 Pore volume, PV 1.6 to 3.4 ml/g Silanol group density (V2 = 6 to 20 ml NaOH consumption) Average aggregate size 250 to 1500 nm CTAB surface area 30 to 350 m.sup.2 /g DBP value 150 to 300 ml/100 g V.sub.2 /V.sub.1 by Hg porosimetry 0.19 to 0.46 DBP/CTAB 1.2 to 2.4. ______________________________________ is produced by reacting alkali silicate with mineral acids at temperatures of 60.degree. to 95.degree. C. while maintaining a pH of 7.5 to 10.5 and continuously stirring, continuing the reaction to a solids concentration in the precipitation suspension of 90 to 120 g/l, adjusting the pH value to a value of less than or equal to 5, filtering out, washing, drying and optionally grinding or granulating the precipitated silica. The precipitated silica is used as a filler in vulcanizable rubber compounds and vulcanizates.

    摘要翻译： 具有以下物理化学性质的沉淀二氧化硅：BET表面积35至350m 2 / g-BET / CTAB表面积比0.8至1.1-孔体积，PV 1.6至3.4ml / g - 硅烷醇密度（V2 = 6至20 ml - NaOH消耗） - 平均骨料大小250至1500nm - CTAB表面积30至350m 2 / g - DBP值150至300ml / 100g -V2 / V1通过Hg孔隙率法0.19至0.46-DBP / CTAB 1.2至2.4 。 - 通过使碱性硅酸盐与无机酸在60℃至95℃的温度下反应，同时保持pH为7.5至10.5并连续搅拌，将反应持续至90至120g / l的沉淀悬浮液中的固体浓度 ，将pH值调节至小于或等于5的值，过滤，洗涤，干燥和任选研磨或造粒沉淀二氧化硅。 沉淀二氧化硅用作可硫化橡胶化合物和硫化橡胶中的填料。

    Precipitated silica
    4.
    发明申请
    Precipitated silica 审中-公开

    公开(公告)号：US20050282951A1

    公开(公告)日：2005-12-22

    申请号：US11194481

    申请日：2005-08-02

    申请人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    发明人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    IPC分类号： C01B33/193 ,  C08K3/36 ,  C08K3/34

    CPC分类号： C01B33/193 ,  B60C1/0016 ,  C01P2004/50 ,  C01P2004/61 ,  C01P2004/62 ,  C01P2006/12 ,  C01P2006/14 ,  C01P2006/19 ,  C08K3/36 ,  Y10T428/2982 ,  C08L21/00

    摘要： A precipitated silica with the following physicochemical properties: BET surface area35 m2/g to 350 m2/g BET/CTAB surface area ratio0.8 to 1.1 Pore volume, PV1.6 ml/g to 3.4 ml/g Silanol group density3 ml/(1.5 g) to 9.5 ml/(1.5 g) (V2 = NaOH consumption) Average aggregate size250 nm to 1500 nm CTAB surface area30 m2/g to 350 m2/g DBP value150 ml/100 g to 300 ml/100 g V2/V1 by Hg porosimetry0.19 to 0.46 DBP/CTAB1.2 to 3.5 is produced by reacting alkali silicate with mineral acids at temperatures of 60° C. to 95° C. while maintaining a pH of 7.5 to 10.5 and continuously stirring, continuing the reaction to a solids concentration in the precipitation suspension of 90 g/l to 120 g/l, adjusting the pH value to a value of less than or equal to 5, filtering out, washing, drying and optionally grinding or granulating the precipitated silica. The precipitated silica is used as a filler in vulcanizable rubber compounds and vulcanizates.

    Precipitated silicas
    5.
    发明授权
    Precipitated silicas 失效

    公开(公告)号：US06977065B1

    公开(公告)日：2005-12-20

    申请号：US08870591

    申请日：1997-06-06

    申请人： Heinz Esch ,  Udo Görl ,  Robert Kuhlmann ,  Ralf Rausch

    发明人： Heinz Esch ,  Udo Görl ,  Robert Kuhlmann ,  Ralf Rausch

    IPC分类号： C01B33/193 ,  C08K3/36 ,  C01B33/12

    CPC分类号： C01B33/193 ,  B60C1/0016 ,  C01P2004/50 ,  C01P2004/61 ,  C01P2004/62 ,  C01P2006/12 ,  C01P2006/14 ,  C01P2006/19 ,  C08K3/36 ,  Y10T428/2982 ,  C08L21/00

    摘要： A precipitated silica with the following physicochemical properties: BET surface area35 m2/g to 350 m2/g BET/CTAB surface area ratio0.8 to 1.1 Pore volume, PV1.6 ml/g to 3.4 ml/g Silanol group density3 ml/(1.5 g) to 9.5 ml/(1.5 g) (V2 = NaOH consumption) Average aggregate size250 nm to 1500 nm CTAB surface area30 m2/g to 350 m2/g DBP value150 ml/100 g to 300 ml/100 g V2/V1 by Hg porosimetry0.19 to 0.46 DBP/CTAB1.2 to 3.5 is produced by reacting alkali silicate with mineral acids at temperatures of 60° C. to 95° C. while maintaining a pH of 7.5 to 10.5 and continuously stirring, continuing the reaction to a solids concentration in the precipitation suspension of 90 g/l to 120 g/l, adjusting the pH value to a value of less than or equal to 5, filtering out, washing, drying and optionally grinding or granulating the precipitated silica. The precipitated silica is used as a filler in vulcanizable rubber compounds and vulcanizates.

    Precipitated silica
    6.
    发明授权
    Precipitated silica 失效
    沉淀二氧化硅

    公开(公告)号：US5871867A

    公开(公告)日：1999-02-16

    申请号：US954858

    申请日：1997-10-21

    申请人： Ralf Rausch ,  Heinz Esch ,  Robert Kuhlmann ,  Guenter Tuerk ,  Karl Meier ,  Walter Meon

    发明人： Ralf Rausch ,  Heinz Esch ,  Robert Kuhlmann ,  Guenter Tuerk ,  Karl Meier ,  Walter Meon

    IPC分类号： C01B33/143 ,  C01B33/18 ,  C01B33/193 ,  C08K3/36 ,  C08L23/06 ,  H01M2/14 ,  H01M2/16

    CPC分类号： H01M2/14 ,  C01B33/193 ,  H01M2/1646 ,  C01P2004/51 ,  C01P2004/61 ,  C01P2006/12 ,  C01P2006/19 ,  C01P2006/80 ,  C01P2006/82

    摘要： Precipitated silica with a sodium sulphate content of 4 to 18 wt. %, particularly with the physical-chemical data:______________________________________Sodium sulphate content: 4-14 wt. %BET surface area (DIN 66131): 100-190 m.sup.2 /gDBP absorption (anhydrous) 208-250 g/100 g(DIN 53601, ASTM D 2414): 3.0-6.5 wt. %(DIN ISO 787/II)Oversize with >63 .mu.m .ltoreq. 10.0 wt. %ALPINE air-jet sieve >150 .mu.m .ltoreq. 0.1 wt. % >250 .mu.m .ltoreq. 0.01 wt. %______________________________________It is prepared by introducing hot water into a precipitation vessel, with stirring, adding water glass, then heating the mixture and maintaining the temperature throughout the remainder of the precipitation period. Water glass and sulphuric acid are added simultaneously during this process. The precipitated silica is then separated from the suspension and the filter cake containing sodium sulphate is dried in a spray drier and ground. The precipitated silica may be used in the production of battery separators.

    摘要翻译： 硫酸钠含量为4〜18重量％的沉淀二氧化硅 ％，特别是物理化学数据： - 硫酸钠含量：4-14重量％ ％ - BET表面积（DIN 66131）：100-190m2 / g-DBP吸收（无水）208-250g / 100g - （DIN 53601，ASTM D 2414）：3.0-6.5wt。 ％ - （DIN ISO 787 / II） - >63μm超大，10.0wt。 ％ - ALPINE喷气筛>150μm0.1重量％ ％ - >250μm<0.01wt。 ％ - 通过将热水引入沉淀容器中，在搅拌下加入水玻璃，然后加热混合物并在整个沉淀期的剩余时间内保持温度而制备。 在此过程中同时加入水玻璃和硫酸。 然后将沉淀的二氧化硅与悬浮液分离，并将含有硫酸钠的滤饼在喷雾干燥器中干燥并研磨。 沉淀二氧化硅可用于生产电池隔板。

    Precipitated Silica
    8.
    发明申请
    Precipitated Silica 审中-公开

    公开(公告)号：US20070208127A1

    公开(公告)日：2007-09-06

    申请号：US11536505

    申请日：2006-09-28

    申请人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    发明人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    IPC分类号： C01B33/14 ,  C08L21/00

    CPC分类号： C01B33/193 ,  B60C1/0016 ,  C01P2004/50 ,  C01P2004/61 ,  C01P2004/62 ,  C01P2006/12 ,  C01P2006/14 ,  C01P2006/19 ,  C08K3/36 ,  Y10T428/2982 ,  C08L21/00

    摘要： A precipitated silica with the following physiochemical properties: BET surface area35 m2/g to 350 m2/g BET/CTAB surface area ratio0.8 to 1.1 Pore volume, PV1.6 ml/g to 3.4 ml/g Silanol group density (V2 = NaOH3 ml/(1.5 g) to 9.5 ml/(1.5 g) consumption) Average aggregate size250 nm to 1500 nm CTAB surface area30 m2/g to 350 m2/g DBP value150 ml/100 g to 300 ml/100 g V2/V1 by Hg porosimetry0.19 to 0.46 DBP/CTAB1.2 to 3.5 is produced by reacting alkali silicate with mineral acids at temperatures of 60° C. to 95° C. while maintaining a pH of 7.5 to 10.5 and continuously stirring, continuing the reaction to a solids concentration in the precipitation suspension of 90 g/l to 120 g/l, adjusting the pH value to a value of less than or equal to 5, filtering out, washing, drying and optionally grinding or granulating the precipitated silica. The precipitated silica is used as a filler in vulcanizable rubber compounds and vulcanizates.

    Precipitated silicas
    9.
    发明授权
    Precipitated silicas 失效
    沉淀二氧化硅

    公开(公告)号：US5925708A

    公开(公告)日：1999-07-20

    申请号：US893225

    申请日：1997-07-15

    申请人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    发明人： Heinz Esch ,  Udo Gorl ,  Robert Kuhlmann ,  Ralf Rausch

    IPC分类号： C01B33/193 ,  C08K3/00

    CPC分类号： C01B33/193 ,  C01P2004/50 ,  C01P2004/61 ,  C01P2004/62 ,  C01P2006/12 ,  C01P2006/14 ,  C01P2006/19

    摘要： A precipitated silica with the following physicochemical properties:______________________________________BET surface area 35 to 350 m.sup.2 /gBET/CTAB surface area ratio 0.8 to 1.1Pore volume, PV 1.6 to 3.4 ml/gSilanol group density (V2 = 6 to 20 mlNaOH consumption)Average aggregate size 250 to 1500 nmCTAB surface area 30 to 350 m.sup.2 /gDBP value 150 to 300 ml/100 gV.sub.2 /V.sub.1 by Hg porosimetry 0.19 to 0.46DBP/CTAB 1.2 to 2.4.______________________________________is produced by reacting alkali silicate with mineral acids at temperatures of 60 to 95.degree. C. while maintaining a pH of 7.5 to 10.5 and continuously stirring, continuing the reaction to a solids concentration in the precipitation suspension of 90 to 120 g/l, adjusting the pH value to a value of less than or equal to 5, filtering out, washing, drying and optionally grinding or granulating the precipitated silica. The precipitated silica is used as a filler in vulcanizable rubber compounds and vulcanizates.

    摘要翻译： 具有以下物理化学性质的沉淀二氧化硅：BET表面积35至350m 2 / g-BET / CTAB表面积比0.8至1.1-孔体积，PV 1.6至3.4ml / g - 硅烷醇密度（V2 = 6至20 ml - NaOH消耗） - 平均骨料大小250至1500nm - CTAB表面积30至350m 2 / g - DBP值150至300ml / 100g - 通过Hg孔隙率法的V2 / V1 0.19至0.46-DBP / CTAB 1.2至2.4 。 - 通过使碱性硅酸盐与无机酸在60至95℃的温度下反应，同时保持pH为7.5至10.5并连续搅拌，将反应持续至90至120g / l的沉淀悬浮液中的固体浓度， 将pH值调节至小于或等于5的值，过滤，洗涤，干燥和任选研磨或造粒沉淀二氧化硅。 沉淀二氧化硅用作可硫化橡胶化合物和硫化橡胶中的填料。