US3948676A
Expired / Lapsed
US
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Process for preparing hydrophobic particles
Assignee: Evonik Operations GmbH
•
Filing: 1974-05-23
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Granted: 1976-04-06
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Expires: 1994-05-23
Abstract
Abstract A process for preparing hydrophobic finely divided oxides of metals and/or oxides of silicon comprising activating finely divided particles of oxides of metals and/or oxides of silicon by heating the particles at about 700° - 1000°C for less than about 60 seconds in a stream of inert gas to substantially completely free the particles of not only the physically bonded, but also the chemically bonded water, and contacting the activated particles with at least one organosilicon compound and substantially anhydrous ammonia gas for less than about 60 seconds. The hydrophobic products are useful as fillers in elastomers.
Inventors
- 👤 Siegmar Laufer
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 10:13
CPC Classifications
C; C09; C09C; C09C3/00; C09C3/12; C01; C01B; C01B13/00; C01B13/14; C01B13/145; C01B33/00; C01B33/113; C08; C08K; C08K9/00; C08K9/04; C08K9/06; C09C1/00; C09C1/28; C09C1/30; C09C1/3081; C09C1/309; C09C3/006; C01P; C01P2006/00; C01P2006/12; C01P2006/20; C01P2006/80; C01P2006/90
Claims Analysis
Total Claims: 50
Claim 1
Independent Claim
92 words
A process for preparing hydrophobic finely divided oxides of metals or oxides of silicon comprising activating finely divided particles of oxides of metals, oxides of silicon or mixtures of these oxides by heating the particles at about 700° - 1000°C for less than about 60 seconds in a stream of inert gas to completely free the particles of physically adsorbed and chemically bonded water, contacting the activated particles with at least one organosilicon compound and anhydrous ammonia gas for less than about 60 seconds at a temperature of about 20° - 100°C.
Claim 2
Dependent Claim
92 words
A process for preparing hydrophobic finely divided oxides of metals or oxides of silicon comprising activating finely divided particles of oxides of metals, oxides of silicon or mixtures of these oxides by heating the particles at about 700° - 1000°C for less than about 60 seconds in a stream of inert gas to completely free the particles of physically adsorbed and chemically bonded water, contacting the activated particles with at least one organosilicon compound and anhydrous ammonia gas for less than about 60 seconds at a temperature of about 20° - 100°C.
Claim 3
Dependent Claim
22 words
Process of claim 1 in which the activated particles are first contacted with the ammonia gas, then contacted with the organosilicon compound.
Claim 4
Dependent Claim
22 words
Process of claim 1 in which the activated particles are first contacted with the organosilicon compound then contacted with the ammonia gas.
Claim 5
Dependent Claim
19 words
Process of claim 1 in which the activated particles are contacted with the organosilicon compound and ammonia gas simultaneously.
Claim 6
Dependent Claim
14 words
Process of claim 1 in which the particles are activated in a fluidized bed.
Claim 7
Dependent Claim
25 words
Process of claim 1 operated on a continuous basis by continuously contacting the oxide particles with the organosilicon compound and ammonia in a fluidized bed.
Claim 8
Dependent Claim
58 words
Process of claim 1 in which the organosilicon compound is an organoalkoxy silane of the formula: R.sub.n Si (OR') .sub.4-n in which R is an alkyl radical having 1 - 12 carbon atoms or an aryl radical, and R' is an alkyl radical having 1 - 8 carbon atoms, and n is the integer 1, 2 or 3.
Claim 9
Dependent Claim
44 words
Process of claim 7 in which the organoalkoxy silane has the formula: R.sub.2 Si (OR').sub.2 in which R is an alkyl radical having 1 - 8 carbon atoms or an aryl radical, and R' is an alkyl radical having 1 - 8 carbon atoms.
Claim 10
Dependent Claim
44 words
Process of claim 7 in which the organoalkoxy silane has the formula: R - Si (OR').sub.3 wherein R is an alkyl radical having 1 - 12 carbon atoms or an aryl radical, and R' is an alkyl radical having 1 - 8 carbon atoms.
Claim 11
Dependent Claim
67 words
Process of claim 1 in which the organosilicon compound is an organoalkoxy siloxane or an organoalkoxy-oligo siloxane of the formula: ##EQU8## wherein X is R or OR', Y is R of OR', R is an alkyl radical having 1 - 8 carbon atoms or an aryl radical, and R' is an alkyl radical having 1 - 8 carbon atoms, and n is the number 0 or 1.
Claim 12
Dependent Claim
57 words
Process of claim 1 in which the organosilicon compound is an organoalkoxy siloxane or an organoalkoxy polysiloxane of the formula: ##EQU9## wherein R is an alkyl radical having 1 - 8 carbon atoms or an aryl radical, R' is an alkyl radical having 1 - 8 carbon atoms, and n is the number 0, 1 or 2.
Claim 13
Dependent Claim
52 words
Process of claim 10 in which the organoalkoxy siloxane or organoalkoxy-oligo siloxane has the formula: ##EQU10## wherein R is an alkyl radical having 1 - 12 carbon atoms or an aryl radical, and R' is an alkyl radical having 1 - 8 carbon atoms, and n is the number 0 or 1.
Claim 14
Dependent Claim
53 words
Process of claim 1 in which the organosilicon compound is an organoalkoxy cyclosiloxane of the formula: ##EQU11## wherein R is an alkyl radical having 1 - 12 carbon atoms or an aryl radical, and R' is an alkyl radical having 1 - 8 carbon atoms and n is the number 3 or 4.
Claim 15
Dependent Claim
34 words
Process of claim 7 in which the sum of the number of carbon atoms in any radical R plus the number of carbon atoms in any other radical R' does not substantially exceed 9.
Claim 16
Dependent Claim
12 words
Process of claim 14 in which the sum is 9 or less.
Claim 17
Dependent Claim
34 words
Process of claim 11 in which the sum of the number of carbon atoms in any radical R plus the number of carbon atoms in any other radical R' does not substantially exceed 9.
Claim 18
Dependent Claim
12 words
Process of claim 16 in which the sum is 9 or less.
Claim 19
Dependent Claim
34 words
Process of claim 12 in which the sum of the number of carbon atoms in any radical R plus the number of carbon atoms in any other radical R' does not substantially exceed 9.
Claim 20
Dependent Claim
12 words
Process of claim 18 in which the sum is 9 or less.
Claim 21
Dependent Claim
28 words
Process of claim 14 in which either the radical R or the radical R' in the organoalkoxy silane has as large a number of carbon atoms as possible.
Claim 22
Dependent Claim
27 words
Process of claim 14 in which the R of the organoalkoxy silane has 3 - 8 carbon atoms and the R' has 1 - 3 carbon atoms.
Claim 23
Dependent Claim
23 words
Process of claim 14 in which the R of the organoalkoxy silane has 6 - 8 carbon atoms and the R' is methyl.
Claim 24
Dependent Claim
44 words
Process of claim 1 in which the organosilicon compound is an organosiloxane of the general formula: ##EQU12## wherein R is CH 3 , an alkyl radical with 2 - 4 carbon atoms or an aryl radical, and n is the number 0 - 8.
Claim 25
Dependent Claim
10 words
Process of claim 23 in which the organosiloxane is hexamethyl-disiloxane.
Claim 26
Dependent Claim
31 words
Process of claim 1 in which the organosilicon compound is an organocyclosiloxane of the formula: ##EQU13## wherein R is CH 3 and n is a number selected from 3 - 10.
Claim 27
Dependent Claim
14 words
Process of claim 1 in which octamethyl-cyclotetrasiloxane (D 4 ) is the organosilicon compound.
Claim 28
Dependent Claim
21 words
Process of claim 1 in which the organosilicon compound is an organoalkoxy silane, an organoalkoxy polysiloxane, an organosiloxane, or an organo-cyclo-siloxane.
Claim 29
Dependent Claim
20 words
Process of claim 27 in which the organosilicon compound is mixed with the oxides at a temperature above about 20°C.
Claim 30
Dependent Claim
11 words
Process of claim 28 in which mixtures of oxides are treated.
Claim 31
Dependent Claim
17 words
Process of claim 28 in which oxides are gassed at ambient temperature with anhydrous NH 3 .
Claim 32
Dependent Claim
17 words
Process of claim 29 in which oxides are gassed at ambient temperature with anhydrous NH 3 .
Claim 33
Dependent Claim
31 words
Process of claim 27 in which the organosilicon compound is mixed with the oxides at standard pressure and ambient temperature, and the resulting mixture is gassed with anhydrous NH 3 .
Claim 34
Dependent Claim
16 words
Process of claim 27 in which the oxide is precipitated silicic acid or pyrogenic silicic acid.
Claim 35
Dependent Claim
17 words
Process of claim 5 in which the activated particles are contacted with ammonia gas immediately after activation.
Claim 36
Dependent Claim
17 words
Process of claim 25 in which oxides are gassed immediately behind the activation zone with anhydrous ammonia.
Claim 37
Dependent Claim
17 words
Process of claim 26 in which oxides are gassed immediately behind the activation zone with anhydrous ammonia.
Claim 38
Dependent Claim
13 words
Process of claim 7 in which the aryl radical is phenyl or naphthyl.
Claim 39
Dependent Claim
13 words
Process of claim 8 in which the aryl radical is phenyl or naphthyl.
Claim 40
Dependent Claim
13 words
Process of claim 9 in which the aryl radical is phenyl or naphthyl.
Claim 41
Dependent Claim
13 words
Process of claim 10 in which the aryl radical is phenyl or naphthyl.
Claim 42
Dependent Claim
90 words
A continuous process for preparing hydrophobic finely divided oxides of silicon, said process comprising activating finely divided particles of precipitated silicic acid, pyrogenic silicic acid or mixtures thereof by heating said particles at about 700° - 1000°C for less than about 60 seconds in a stream of inert gas to completely free the particles of physically adsorbed and chemically bonded water, and contacting the resulting activated particles with at least one organosilicon compound and anhydrous gas for less than about 60 seconds at a temperature of about 20° - 100°C.
Claim 43
Dependent Claim
90 words
A continuous process for preparing hydrophobic finely divided oxides of silicon, said process comprising activating finely divided particles of precipitated silicic acid, pyrogenic silicic acid or mixtures thereof by heating said particles at about 700° - 1000°C for less than about 60 seconds in a stream of inert gas to completely free the particles of physically adsorbed and chemically bonded water, and contacting the resulting activated particles with at least one organosilicon compound and anhydrous gas for less than about 60 seconds at a temperature of about 20° - 100°C.
Claim 44
Dependent Claim
20 words
Process of claim 41 in which the activated particles, organosilicon compound and anhydrous ammonia gas are contacted at standard pressure.
Claim 45
Dependent Claim
20 words
Process of claim 42 in which the activated particles, organosilicon compound and anhydrous ammonia gas are contacted at ambient temperature.
Claim 46
Dependent Claim
23 words
Process of claim 42 in which the activated particles, organosilicon compound and anhydrous ammonia gas are contacted at a temperature above about 20°C.
Claim 47
Dependent Claim
43 words
Process of claim 43 in which the organosilicon compound is linear hexamethyl-cyclotrisiloxane (D 2 ), cyclic hexamethyl-cyclotrisiloxane (D 3 ), octamethyl-cyclotetrasiloxane (D 4 ), hexamethyl-disiloxane n-propyl-triisopropyl silane, a mixture of C 6 -C 8 alkyl trimethoxysilane, n-propyl-tris-2-ethylhexoxy silane, n-propyl-n-butoxy silane, and di-n-propyl-tetra-n-butoxy disilane.
Claim 48
Dependent Claim
43 words
Process of claim 1 in which the organosilicon compound is linear hexamethyl-cyclotrisiloxane (D 2 ), cyclic hexamethyl-cyclotrisiloxane (D 3 ), octamethyl-cyclotetrasiloxane (D 4 ), hexamethyl-disiloxane, n-propyl-triisopropyl silane, a mixture of C 6 -C 8 alkyl trimethosysilane, n-propyl-tris-2-ethylhexoxy silane, n-propyl-n-butoxy silane, and di-n-propyl-tetra-n-butoxy disilane.
Claim 49
Dependent Claim
21 words
Process of claim 41 in which said activated particles are contacted with the ammonia gas and organosilicon compound at atmospheric pressure.
Claim 50
Dependent Claim
28 words
Process of claim 41 in which said activated particles are contacted with the ammonia gas and organosilicon compound at about 10 - 3 to about 10 3 torr.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-04-06 | 1979-10-06 | 1980-04-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-04-06 | 1983-10-06 | 1984-04-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-04-06 | 1987-10-06 | 1988-04-06 | $7700.00 | Window Closed / Lapsed |