CN101304946A - 干液体、制备干液体的方法和设备 - Google Patents
干液体、制备干液体的方法和设备 Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/112—Stirrers characterised by the configuration of the stirrers with arms, paddles, vanes or blades
- B01F27/1122—Stirrers characterised by the configuration of the stirrers with arms, paddles, vanes or blades anchor-shaped
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/84—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with two or more stirrers rotating at different speeds or in opposite directions about the same axis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/93—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with rotary discs
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
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Abstract
本发明涉及干液体及其制备方法和制备设备。在本发明方法中,通过高强度搅拌器混合液体和疏水二氧化硅来制备各个液滴尺寸小于5μm的包含疏水的热解制备的二氧化硅的干液体,壁-沟流搅拌器同时运动并且所述高强度搅拌器在其轴向上运动。
Description
本发明涉及干液体、制备干液体(dry liquid)的方法和设备。
US 3,393,155中公开了干液体,特别是干水(dry water)。
它们包含平均粒径不超过50毫微米、表面具有疏水性的热解制备的二氧化硅,并且它们包含5-10倍的微囊剂形式(encapsulated form)的液体。
尽管大部分是水,但是粉末(干水)具有粉状的外观。
可以通过将液体分成细的液滴并且使用高能输入将这些细的液滴与斥水的热解制备的二氧化硅混合,使得液滴完全被斥水的二氧化硅所包围来制备已知的干粉(US 3,393,155)。
此外,已知可以通过在高剪切条件下使水与疏水的热解制备的二氧化硅混合并结合来制备钻井液(drilling fluid)组分,获得可流动的、干的、粉状的固体产品。
可以在高剪切条件下进行混合。因此,在实验室中可以使用高速泵或者分散器。在较大规模上,可以使用具备叶片的旋转搅拌器、适于向混合物引入高剪切能的混合泵或者任何其它混合器(US 3,951,824)。
此外,已知干水可以通过与水一起搅拌二氧化硅来制备并且可以用作灭火剂。干水可以在低温下储存,因为既使在非常低的温度下它也不会作为粉末丧失其流动性(US 5,342,597和US 4,008,170)。
此外,已知干水还可以通过使用“摇动混合器”或者振荡设备作为使混合物高速运动的设备来制备(US 2004/0028710 A1)。
已知的方法的缺点在于都只能制备相对少量的干水。
此外,已知的干液体都只具有有限的储存稳定性。
因此,本发明目的是开发一种不具有所述缺点的干液体。另外,打算开发一种可以制备较大量干水的方法。
本发明涉及包含疏水的热解制备的二氧化硅的干液体,其特征在于各个液滴尺寸小于5μm。
优选,各个液滴尺寸可以在1-4.5μm的范围内。
本发明还涉及包含疏水的热解制备的二氧化硅的干液体,其特征在于下面的物理化学参数:
粒径分布(团块尺寸分布)
(累积筛下物)
D10% 80-140μm
D50% 140-200μm
D90% 190-340μm
堆积密度DIN 53912 kg/m3 400-500
夯实密度DIN ISO 787kg/m3 500-600
固体含量DIN 53 198% 4-10。
本发明还涉及干液体的制备方法,其特征在于将所述液体和疏水的热解制备的二氧化硅引入容器中并且通过高强度搅拌器在那里混合,壁-沟流搅拌器(wall-channelling stirrer)同时运动和高强度搅拌器在其轴向上运动。
根据本发明,通过高强度搅拌器,任选地通过剪切产生液滴。
使这些液滴与疏水的热解制备的二氧化硅接触。搅拌器可以是壁-沟流慢旋转搅拌器,通过该搅拌器,将材料从不会发生由高强度搅拌器混合的盲区(dead zone)传输到高强度搅拌器的剪切区域。
通过轴向运动,举例来说如向上和向下运动,可以保证在轴向上发生彻底的混合。
容器可以是圆柱状、球状、具备圆锥的圆柱状或者具备球形的圆柱状。
可以使用齿-盘搅拌器作为高强度搅拌器。
液体应理解为意指水、盐的水溶液、甘油的水溶液和药剂、化妆品等中的相似的水可混溶的液体组分。
本发明还涉及实施所述干液体制备方法的设备,其特征在于它包括高强度搅拌器(1)、容器(3)和壁-沟流搅拌器(10),布置所述高强度搅拌器(1),使之在轴向上可以运动。
本发明的优点在于开发了具有良好储存稳定性的干液体。
附图说明
图1所示为根据本发明的干液体制备设备。
图2所示为各个液滴的尺寸与圆周速度的关系。
下面参照附图更详细地解释并说明根据本发明的方法和根据本发明的设备。
根据图1,作为高强度搅拌器在12-45rn/s的圆周速度下操作齿-盘搅拌器1。齿-盘搅拌器1具有锯齿盘2并且顺时针方向旋转。容器3具有圆柱形部分4和圆锥形部分5。圆柱4与圆锥5的直径比为1至0.3。圆锥5与高强度搅拌器的比例为0.9至0.3。圆柱4的高度与直径比为1至2。圆锥5的高度与直径比为1至3。
高强度搅拌器1的旋转导致下面的运动和产物流:
-··-··-··-·· 径向产物流(6)
……………………………… 轴向产物流(7)
------- 高强度混合装置的运动(8)
-·-·-·-·-· 清洗臂的运动(9)
产物流6和7由高强度搅拌器1的旋转产生,从运动(movement)8的角度上看它可以是轴向的,即竖直运动。
当只在一个竖直面中单独操作高强度搅拌器1时,因为液滴的形成随着粉末形成的增加而改变,所以在容器壁上形成水的局部积聚。由于变化的流动特性,形成盲区。
壁-沟流锚式搅拌器(wall-channelling anchor stirrer)10的清洗壁的运动9阻止形成水的局部积聚和盲区。发生均匀的彻底混合。锚式搅拌器10的清洗壁的运动可以是0.2-2m/s。
实施例
使用如图1所示的根据本发明的设备制备干液体:
每种条件表示在表1中:
各个液滴的尺寸与圆周速度的关系以图片表示在图2中。
通过对冷冻干燥的(冷冻制备的)干液体进行TEM分析(bred分析)确定各个液滴的粒径。
如下进行冷冻制备。
在冷冻制备中,首先用液氮将冷冻制备室冷却至大约100K。当打开制备室时,热量使N2蒸发,从而在干N2气氛中进行制备。通过将液N2引入持器的杜瓦瓶中,将制剂持器(preparation holder)同样冷却至大约100K。
对于制剂1,将“干水”撒到涂有薄聚合物层的制备载体网上并且放到冷却至低温的制备室中的一片滤纸上并且冷冻。
对于制剂2,在铜容器中液化乙烷。将撒有“干水”的小片网浸入所述乙烷中。由于液化乙烷较高的热容量,通常水会被突然冷冻成无定形形式,这与制剂1的情况形成对照。与制剂1相比,样品在冷却时不会再改变。
然后,将冷冻的制剂转移到制剂持器中,并且转移到透射电子显微镜中。因为持器被冷却至低温,所以在TEM中可以在冷冻状态下分析制剂。
通过购自RETSCH GmbH & Co.KG,D-42781Haan的Camsizer确定团块的粒径分布。
Claims (4)
1.包含疏水的热解制备的二氧化硅的干液体,其特征在于各个液滴尺寸小于5μm。
2.根据权利要求1的包含疏水的热解制备的二氧化硅的干液体,其特征在于下面的物理化学参数:
粒径分布(团块尺寸分布)(累积筛下物)
D10% 80-140μm
D50% 140-200μm
D90% 190-340μm
堆积密度DIN 53912 kg/m3 400-500
夯实密度DIN ISO 787 kg/m3 500-600
固体含量DIN 53198 % 4-10。
3.根据权利要求1或2的干液体的制备方法,其特征在于将液体和疏水的热解制备的二氧化硅引入容器中并且通过高强度搅拌器在那里混合,壁-沟流搅拌器同时运动并且所述高强度搅拌器在其轴向上运动。
4.实施根据权利要求3的方法的设备,其特征在于它由高强度搅拌器(1)、容器(3)和搅拌器(10)组成,布置所述高强度搅拌器(1),使之在轴向上可以运动。
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CN201510173748.6A CN104828833A (zh) | 2005-11-16 | 2006-10-12 | 干液体、制备干液体的方法和设备 |
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EP05025001.8 | 2005-11-16 | ||
EP05025001A EP1787957A1 (de) | 2005-11-16 | 2005-11-16 | Trockene Flüssigkeiten, Verfahren und Vorrichtung zu ihrer Herstellung |
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CNA2006800416839A Pending CN101304946A (zh) | 2005-11-16 | 2006-10-12 | 干液体、制备干液体的方法和设备 |
CN201510173748.6A Pending CN104828833A (zh) | 2005-11-16 | 2006-10-12 | 干液体、制备干液体的方法和设备 |
CNA2006101603016A Pending CN101070160A (zh) | 2005-11-16 | 2006-11-16 | 干液体、制备干液体的方法和设备 |
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CNA2006101603016A Pending CN101070160A (zh) | 2005-11-16 | 2006-11-16 | 干液体、制备干液体的方法和设备 |
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EP (2) | EP1787957A1 (zh) |
JP (1) | JP5204658B2 (zh) |
CN (3) | CN101304946A (zh) |
WO (1) | WO2007057262A1 (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101863483A (zh) * | 2010-06-18 | 2010-10-20 | 华南理工大学 | 一种合成气体水合物的干水及其制备方法和应用 |
CN101922609A (zh) * | 2010-07-09 | 2010-12-22 | 华南理工大学 | 一种能快速可逆储气的凝胶干水及其制法和应用 |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
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EP2415829A1 (de) | 2010-07-30 | 2012-02-08 | Schaefer Kalk GmbH & Co. KG | Trockene Flüssigkeit |
DE102011077298A1 (de) * | 2011-06-09 | 2012-12-13 | Evonik Degussa Gmbh | Kern-Hülle-Partikel mit einem hohen Gehalt an Glycerin, ihre Herstellung und Verwendung |
WO2013042069A1 (en) * | 2011-09-22 | 2013-03-28 | Ariel-University Research And Development Company, Ltd. | Emulsions and methods of making emulsions |
CN103007479B (zh) * | 2012-12-31 | 2015-04-01 | 西安科技大学 | 一种灭火剂 |
CN103007478B (zh) * | 2012-12-31 | 2015-03-25 | 西安科技大学 | 一种灭火剂及其制备方法 |
CN104785291A (zh) * | 2015-04-09 | 2015-07-22 | 山西大学 | 一种pH响应的干水及其制备方法 |
CN105536662B (zh) * | 2015-12-30 | 2017-12-12 | 西安科技大学 | 一种微胶囊的制备方法 |
CN106925162B (zh) * | 2017-04-13 | 2018-06-29 | 江西黑猫炭黑股份有限公司 | 一种应用于白炭黑生产用的三段式双电机搅拌装置 |
SE542958C2 (en) * | 2018-12-17 | 2020-09-22 | Saltx Tech Ab | Heat storage using phase change material coated with nanoparticles |
US20220002165A1 (en) * | 2019-02-28 | 2022-01-06 | Tokuyama Corporation | Silica powder, resin composition, and dispersion |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
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DE1467023A1 (de) | 1964-02-28 | 1969-01-23 | Degussa | Verfahren zur Inkorporierung von Wasser in feinst verteilter Kieselsaeure |
US3951824A (en) | 1973-02-12 | 1976-04-20 | Continental Oil Company | Dry drilling fluid composition |
US4008170A (en) | 1975-11-28 | 1977-02-15 | The United States Of America As Represented By The Secretary Of The Army | Dry water |
CA1197273A (en) * | 1982-08-26 | 1985-11-26 | Edmund J. Janicki | Dry mix for hydration of plaster |
GB9021061D0 (en) * | 1990-09-27 | 1990-11-07 | Unilever Plc | Encapsulating method and products containing encapsulated material |
US5342597A (en) | 1990-11-14 | 1994-08-30 | Cabot Corporation | Process for uniformly moisturizing fumed silica |
DE9420292U1 (de) * | 1994-12-19 | 1996-04-18 | Stelzer Rührtechnik GmbH, 34414 Warburg | Rührwerk |
TWI314865B (zh) * | 2001-01-18 | 2009-09-21 | Shiseido Co Ltd |
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2005
- 2005-11-16 EP EP05025001A patent/EP1787957A1/de not_active Withdrawn
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2006
- 2006-10-12 CN CNA2006800416839A patent/CN101304946A/zh active Pending
- 2006-10-12 JP JP2008540549A patent/JP5204658B2/ja active Active
- 2006-10-12 WO PCT/EP2006/067352 patent/WO2007057262A1/en active Application Filing
- 2006-10-12 CN CN201510173748.6A patent/CN104828833A/zh active Pending
- 2006-10-12 EP EP06807217.2A patent/EP1948564B1/en active Active
- 2006-11-16 CN CNA2006101603016A patent/CN101070160A/zh active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101863483A (zh) * | 2010-06-18 | 2010-10-20 | 华南理工大学 | 一种合成气体水合物的干水及其制备方法和应用 |
CN101922609A (zh) * | 2010-07-09 | 2010-12-22 | 华南理工大学 | 一种能快速可逆储气的凝胶干水及其制法和应用 |
CN101922609B (zh) * | 2010-07-09 | 2012-10-31 | 华南理工大学 | 一种能快速可逆储气的凝胶干水及其制法和应用 |
Also Published As
Publication number | Publication date |
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JP5204658B2 (ja) | 2013-06-05 |
EP1948564A1 (en) | 2008-07-30 |
EP1787957A1 (de) | 2007-05-23 |
EP1948564B1 (en) | 2017-05-10 |
JP2009515801A (ja) | 2009-04-16 |
CN104828833A (zh) | 2015-08-12 |
WO2007057262A1 (en) | 2007-05-24 |
CN101070160A (zh) | 2007-11-14 |
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