DE19961933A1 - Silica having higher density useful for production of dispersions is prepared by hydrophobising pyrogenically produced silica and compacting it - Google Patents
Silica having higher density useful for production of dispersions is prepared by hydrophobising pyrogenically produced silica and compacting itInfo
- Publication number
- DE19961933A1 DE19961933A1 DE1999161933 DE19961933A DE19961933A1 DE 19961933 A1 DE19961933 A1 DE 19961933A1 DE 1999161933 DE1999161933 DE 1999161933 DE 19961933 A DE19961933 A DE 19961933A DE 19961933 A1 DE19961933 A1 DE 19961933A1
- Authority
- DE
- Germany
- Prior art keywords
- silica
- dispersions
- hydrophobising
- compacting
- pyrogenically produced
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3081—Treatment with organo-silicon compounds
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/20—Powder free flowing behaviour
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
Description
Die Erfindung betrifft eine hydrophobe, pyrogen hergestellte Kieselsäure, ein Verfahren zu ihrer Herstellung und ihrer Ver wendung.The invention relates to a hydrophobic, pyrogenically produced Silicic acid, a process for its production and its ver turn.
Es ist bekannt, hydrophile, pyrogen hergestellte Kieselsäure zu verdichten (EP 0 280 854 B1). Nachteiligerweise nimmt mit zunehmender Stampfdichte, beziehungsweise Schüttgewicht die Verdickungswirkung linear ab. Zusätzlich nimmt die Dispergier barkeit mit zunehmender Dichte ab. Dies zeigt sich durch eine unerwünschte Stippenbildung. Eine hydrophile, pyrogen herge stellte Kieselsäure kann daher nach der Verdichtung nur für eine begrenzte Anzahl von Einsatzzwecken verwendet werden.It is known to be hydrophilic, pyrogenic silica to compress (EP 0 280 854 B1). Unfortunately, takes away increasing tamped density, or bulk density Thickening effect decreases linearly. In addition, the disperser availability with increasing density. This is shown by a unwanted specks. A hydrophilic, pyrogenic herge Silica can therefore only be used for compaction a limited number of uses.
Gegenstand der Erfindung ist eine hydrophobe, pyrogen herge stellte Kieselsäure, welche dadurch gekennzeichnet ist, daß sie eine Stampfdichte von 55 bis 200 g/l aufweist.The invention relates to a hydrophobic, pyrogenic Herge provided silica, which is characterized in that it has a tamped density of 55 to 200 g / l.
Bevorzugt kann die Stampfdichte 60 bis 200 g/l betragen.The tamped density can preferably be 60 to 200 g / l.
Ein weiterer Gegenstand der Erfindung ist ein Verfahren zur Herstellung der hydrophoben, pyrogen hergestellten Kieselsäure mit einem Schüttgewicht von 55 bis 200 g/l, welches dadurch gekennzeichnet ist, daß man pyrogen hergestellte Kieselsäure auf bekanntem Wege hydrophobiert und anschließend verdichtet.Another object of the invention is a method for Production of the hydrophobic, pyrogenic silica with a bulk density of 55 to 200 g / l, which thereby is characterized in that pyrogenic silica hydrophobicized in a known manner and then compacted.
Bevorzugt kann die Hydrophobierung mittels halogenfreier Sila ne erfolgen. Der Chlorid-Gehalt der Kieselsäure kann gleich oder unter 100 ppm, bevorzugt 10 bis 100 ppm betragen.Hydrophobization by means of halogen-free sila is preferred ne done. The chloride content of the silica can be the same or below 100 ppm, preferably 10 to 100 ppm.
Die Verdichtung kann mittels eines Walzenverdichters erfolgen. Bevorzugt kann die Verdichtung mittels eines Preßbandfilters gemäß EP 0 280 851 B1 erfolgen.The compaction can be done using a roller compactor. The compression can preferably be carried out using a press belt filter according to EP 0 280 851 B1.
Als hydrophobe, pyrogen hergestellte Kieselsäure können zum
Beispiel die Kieselsäuren:
Aerosil R 812 oder Aerosil R 812S, mit der Gruppierung
-O-Si (CH3)3
Aerosil R 202, Aerosil MS 202, Aerosil MS 202, Aerosil R 106
oder Aerosil R 104, mit der Gruppierung
For example, as hydrophobic, pyrogenically produced silica, the silicas:
Aerosil R 812 or Aerosil R 812S, with the grouping -O-Si (CH 3 ) 3
Aerosil R 202, Aerosil MS 202, Aerosil MS 202, Aerosil R 106 or Aerosil R 104, with the grouping
Aerosil R 805 mit der Gruppierung
Aerosil R 805 with the grouping
verwendet werden.be used.
Die erfindungsgemäße hydrophobe, pyrogene Kieselsäure mit ei
nem Stampfgewicht von 55 bis 200 g/l weist die folgenden Vor
teile auf:
Auf Grund der höheren Stampfdichte sind die Transportkosten
deutlich niedriger.The hydrophobic, pyrogenic silica according to the invention with a tamped weight of 55 to 200 g / l has the following advantages:
Due to the higher tamping density, the transport costs are significantly lower.
Nach der Dispergierung liegt die erfindungsgemäße Kieselsäure in kleineren Aggregaten vor. Das heißt: Die Dispersionen sind feinteiliger, weil die erfindungsgemäße Kieselsäure besser dispergierbar ist.After the dispersion, the silica according to the invention lies in smaller aggregates. That means: The dispersions are more finely divided because the silica according to the invention is better is dispersible.
Die mit der erfindungsgemäßen Kieselsäure hergestellten Dis persionen weisen einen kleineren Grindometerwert auf.The Dis produced with the silica according to the invention Persions have a smaller grindometer value.
Sowohl die Transparenz, gemessen an UV-Transmission, als auch die visuelle Durchsichtigkeit der Dispersionen werden durch die Verwendung der erfindungsgemäßen Kieselsäure deutlich ver bessert.Both the transparency, measured by UV transmission, as well the visual transparency of the dispersions are through the use of the silica according to the invention clearly ver improves.
Die Dispersionen, die die erfindungsgemäße Kieselsäuren ent halten, zeigen eine deutlich erhöhte Stabilität, weil die Se dimentationsneigung deutlich geringer ist.The dispersions containing the silicas according to the invention hold show a significantly increased stability because the Se tendency to dimentation is significantly lower.
Ein weiterer Vorteil der erfindungsgemäßen Kieselsäure ist die reduzierte Staubbildung bei der Einarbeitung und die deutlich herabgesetzte Einarbeitungs- beziehungsweise Benetzungszeit in zum Beispiel flüssige Systemen.Another advantage of the silica according to the invention is that reduced dust formation during incorporation and the significantly reduced familiarization or wetting time in for example liquid systems.
Die Hydrophobie ist bei der erfindungsgemäßen Kieselsäure ge genüber der hydrophoben, pyrogenen Kieselsäure mit niedrigerem Schüttgewicht unverändert. Auch die Verdickungswirkung ist un verändert.The hydrophobicity of the silica according to the invention is ge compared to the hydrophobic, pyrogenic silica with lower Bulk weight unchanged. The thickening effect is also un changed.
Es werden verschiedene hydrophobe, pyrogen hergestellte Kie selsäuren untersucht, wobei verschiedene Verdichtungszustände gegenübergestellt werden.There are various hydrophobic, pyrogenically produced kie investigated selic acids, different compression states be compared.
Es bedeuten:
lose = pulverförmige, unveränderte Kieselsäure
CF = mit Carterfilter verdichtete Kieselsäure
VV 60 = auf eine Stampfdichte von ca. 60 g/l verdichtete
Kieselsäure
VV 90 = auf eine Stampfdichte von ca. 90 g/l verdichtete
KieselsäureIt means:
loose = powdered, unchanged silica
CF = silica compressed with Carter filter
VV 60 = silica compressed to a tamped density of approx. 60 g / l
VV 90 = silica compressed to a tamped density of approx. 90 g / l
Untersucht werden die Aerosil-Typen R 202, US 202, US 204, R 812, R812S und R 805. Die Ergebnisse sind in der Tabelle 1 aufgeführt.The aerosil types R 202, US 202, US 204, R are examined 812, R812S and R 805. The results are shown in Table 1 listed.
Die Methanolbenetzbarkeit zeigt Fig. 3.The methanol wettability is shown in FIG. 3.
Der Verdichtungsgrad hat praktisch keinen nennenswerten Ein fluß auf die Hydrophobie, beurteilt nach der Methanolbenetz barkeit nach Corning Glass. Auch die Viskosität zeigt keine deutliche systematische Abhängigkeit von der Stampfdichte. Insbesondere bei R 812 wird die Dispergierbarkeit mit steigen der Dichte besser. R 812 S. das mehr SiOH-Gruppen enthält als R 812, zeigt obiges Phänomen weniger deutlich.The degree of compression has practically no appreciable one flow on the hydrophobicity, judged by the methanol wetting availability according to Corning Glass. The viscosity also shows none clear systematic dependence on the tamped density. With R 812 in particular, the dispersibility will also increase the density better. R 812 S. which contains more SiOH groups than R 812, shows the above phenomenon less clearly.
US 202 und US 204 sind rheologisch gut miteinander vergleich bar und AEROSIL R 202 unterlegen.US 202 and US 204 are rheologically well compared bar and AEROSIL R 202.
Die verdichteten Varianten zeigen überraschender Weise insbe
sondere bei R 812, R 202 und US 202/4 eine um bis zur Hälfte
verkürzte Einarbeitungszeit. Ferner zeigen die verdichteten
Kieselsäuren eine geringere Staubentwicklung.
The compressed variants surprisingly show, in particular in the case of the R 812, R 202 and US 202/4, a training time which is reduced by up to half. Furthermore, the compressed silicas show less dust.
Die Ergebnisse sind in den Fig. 1, 8 und 4 dargestellt
Rhlogiische Prüfung:
Polymer: Araldit M
Thixmittel: R 202 und R 812
Zusatz: -The results are shown in FIGS . 1, 8 and 4.
Polymer: Araldit M
Thix: R 202 and R 812
Additive: -
Probe A R 812 10 kg 2-10123
Herstellungsdatum der Probe: 24.02.1994 Spindel:5
Sample AR 812 10 kg 2-10123
Date of manufacture of the sample: 24.02.1994 Spindle: 5
Probe A R 812 15 kg 1,0/8 min
Herstellungsdatum der Probe: 24.02.1994 Spindel:5
Sample AR 812 15 kg 1.0 / 8 min
Date of manufacture of the sample: 24.02.1994 Spindle: 5
Probe A R 812 20 kg 0,6/14 min
Herstellungsdatum der Probe: 24.02.1994 Spindel:5
Sample AR 812 20 kg 0.6 / 14 min
Date of manufacture of the sample: 24.02.1994 Spindle: 5
Die Verdichtung kann eine Art Vordispergierung darstellen. Entsprechend erhöhen sich mit der Stampfdichte die Effekti vitätswerte, das heißt die effektiv vorliegenden Teilchen in der Ethanoldispersion werden kleiner und die verdichte ten Proben setzen sich deutlich weniger ab. The compression can be a kind of predispersion. The effect increases accordingly with the tamped density vity values, i.e. the particles actually present in the ethanol dispersion the smaller and the more compact ten samples settle significantly less.
Entsprechend ist in Araldit der Grindometerwert der ver dichteten Proben günstiger. Da die größeren Teilchen aber maßgeblich die Verdickungswirkung beeinflussen, geht diese mit der Verdichtung geringfügig zurück.Accordingly, the grindometer value in araldite is the ver sealed samples cheaper. Since the larger particles significantly affect the thickening effect, this goes with the compression slightly back.
Der Graphik mit den Effektivitätswerten kann man entnehmen, daß die hoch verdichtete AEROSIL R 812-Probe zwar noch mit dem Ultra-Turrax (0965), aber nicht mehr mit dem Dissolver (0955) aufgeschlossen werden kann. Aufgrund der geringeren Oberfläche von AEROSIL R 202 (und der damit prinzipiell besseren Dispergierbarkeit) tritt dieses Phänomen bei AERO- SIL R 202 kaum auf.The graphic with the effectiveness values can be seen that the highly compressed AEROSIL R 812 sample is still included the Ultra-Turrax (0965), but no longer with the dissolver (0955) can be unlocked. Because of the lesser Surface of AEROSIL R 202 (and therefore in principle better dispersibility) this phenomenon occurs with AERO- SIL R 202 barely open.
Mit steigender Verdichtung werden die effektiv vorliegenden Teilchen in einer Ethanoldispersion also kleiner und die Streuung im 90-Grad-Winkel aufgrund der Rayleigh-Streuung größer. Die Totalstreuung (über alle Winkel) wird aber kleiner, die Proben werden für das Auge deutlich transpa renter, was auch die UV-Transmissionsspektren belegen.With increasing compression, the effective ones become Particles in an ethanol dispersion are smaller and that Scattering at a 90 degree angle due to Rayleigh scattering greater. The total scatter (over all angles) is however smaller, the samples become clearly transparent to the eye renter, which is also proven by the UV transmission spectra.
Die Verdichtung hat keinen Einfluß auf die Hydrophbie, die mit der des Standardmusters jeweils weitgehend überein stimmt. The compression has no effect on the Hydrophbie, the largely corresponds to that of the standard sample Right.
Die verdichteten AEROSIL R 202-Proben verhalten sich analog zu den verdichteten AEROSIL R 812-Proben.The compressed AEROSIL R 202 samples behave analogously to the compressed AEROSIL R 812 samples.
Bezüglich der Diskussion wird daher auf Beispiel 2 verwie sen.With regard to the discussion, reference is therefore made to Example 2 sen.
Die Methanolbenetzbarkeit ist in der Fig. 5 graphisch dar gestellt.The methanol wettability is shown graphically in FIG. 5.
Claims (3)
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE1999161933 DE19961933A1 (en) | 1999-12-22 | 1999-12-22 | Silica having higher density useful for production of dispersions is prepared by hydrophobising pyrogenically produced silica and compacting it |
GB0030863A GB2357497A (en) | 1999-12-22 | 2000-12-18 | Hydrophobic silica |
JP2000385876A JP2001226113A (en) | 1999-12-22 | 2000-12-19 | Hydrophobic silica manufactured by thermal decomposition, its manufacturing method and use thereof |
US09/740,039 US20020037936A1 (en) | 1999-12-22 | 2000-12-20 | Hydrophobic silica |
US10/623,051 US7282236B2 (en) | 1999-12-22 | 2003-07-18 | Hydrophobic silica |
US11/741,381 US20070202030A1 (en) | 1999-12-22 | 2007-04-27 | Hydrophobic silica |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE1999161933 DE19961933A1 (en) | 1999-12-22 | 1999-12-22 | Silica having higher density useful for production of dispersions is prepared by hydrophobising pyrogenically produced silica and compacting it |
Publications (1)
Publication Number | Publication Date |
---|---|
DE19961933A1 true DE19961933A1 (en) | 2001-07-26 |
Family
ID=7933751
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE1999161933 Ceased DE19961933A1 (en) | 1999-12-22 | 1999-12-22 | Silica having higher density useful for production of dispersions is prepared by hydrophobising pyrogenically produced silica and compacting it |
Country Status (1)
Country | Link |
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DE (1) | DE19961933A1 (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003054448A1 (en) * | 2001-12-13 | 2003-07-03 | Degussa Ag | Method for separating ashes in combustion installations |
WO2003106602A1 (en) * | 2002-06-14 | 2003-12-24 | Degussa Ag | Cable gels for optical fibre cables |
WO2005054390A1 (en) * | 2003-12-01 | 2005-06-16 | Degussa Ag | Adhesive and sealant systems |
EP1813574A1 (en) * | 2006-01-25 | 2007-08-01 | Degussa GmbH | Sheet compacted pyrogenic silicon dioxide |
WO2007085503A1 (en) * | 2006-01-25 | 2007-08-02 | Evonik Degussa Gmbh | Process for preparation of rubber mixtures containing silicon dioxide |
DE102007059862A1 (en) * | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Through-and-through hydrophobic slugs of pyrogenically produced silicon dioxide |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0010655A1 (en) * | 1978-10-12 | 1980-05-14 | Wacker-Chemie GmbH | Process for increasing the bulk density of silicon dioxide and a use of the so treated silicon dioxide |
EP0280851B1 (en) * | 1987-02-26 | 1991-04-24 | Degussa Aktiengesellschaft | Process for compressing pyrogenic silica |
-
1999
- 1999-12-22 DE DE1999161933 patent/DE19961933A1/en not_active Ceased
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0010655A1 (en) * | 1978-10-12 | 1980-05-14 | Wacker-Chemie GmbH | Process for increasing the bulk density of silicon dioxide and a use of the so treated silicon dioxide |
EP0280851B1 (en) * | 1987-02-26 | 1991-04-24 | Degussa Aktiengesellschaft | Process for compressing pyrogenic silica |
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003054448A1 (en) * | 2001-12-13 | 2003-07-03 | Degussa Ag | Method for separating ashes in combustion installations |
WO2003106602A1 (en) * | 2002-06-14 | 2003-12-24 | Degussa Ag | Cable gels for optical fibre cables |
DE10226520A1 (en) * | 2002-06-14 | 2004-01-08 | Degussa Ag | cable gels |
US7095929B2 (en) | 2002-06-14 | 2006-08-22 | Degussa Ag | Cable gels for optical fibre cables |
WO2005054390A1 (en) * | 2003-12-01 | 2005-06-16 | Degussa Ag | Adhesive and sealant systems |
US8022130B2 (en) | 2003-12-01 | 2011-09-20 | Evonik Degussa Gmbh | Adhesive and sealant systems |
EP1813574A1 (en) * | 2006-01-25 | 2007-08-01 | Degussa GmbH | Sheet compacted pyrogenic silicon dioxide |
WO2007085503A1 (en) * | 2006-01-25 | 2007-08-02 | Evonik Degussa Gmbh | Process for preparation of rubber mixtures containing silicon dioxide |
WO2007085511A1 (en) * | 2006-01-25 | 2007-08-02 | Evonik Degussa Gmbh | Pyrogenically prepared silicon dioxide compacted to give crusts |
US7842269B2 (en) | 2006-01-25 | 2010-11-30 | Evonik Degussa Gmbh | Pyrogenically prepared silicon dioxide compacted to give crusts |
US8252853B2 (en) | 2006-01-25 | 2012-08-28 | Evonik Degussa Gmbh | Process for preparation of rubber mixtures containing silicon dioxide |
DE102007059862A1 (en) * | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Through-and-through hydrophobic slugs of pyrogenically produced silicon dioxide |
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Legal Events
Date | Code | Title | Description |
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OP8 | Request for examination as to paragraph 44 patent law | ||
8127 | New person/name/address of the applicant |
Owner name: DEGUSSA GMBH, 40474 DUESSELDORF, DE |
|
8127 | New person/name/address of the applicant |
Owner name: EVONIK DEGUSSA GMBH, 40474 DUESSELDORF, DE |
|
R002 | Refusal decision in examination/registration proceedings | ||
R003 | Refusal decision now final |
Effective date: 20121221 |