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US5424095A Expired / Lapsed US ⏱️ 0.0 years remaining

Ceramic vapor deposited coating using a steam-containing carrier gas and non-alkoxy silane precursors

Assignee: Eni Tecnologie SpA
•
Filing: 1994-03-07
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Granted: 1995-06-13
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Expires: 2014-03-07
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Abstract

Abstract In order to reduce the rate of coke formation during the industrial pyrolysis of hydrocarbons, the interior surface of a reactor is coated with a uniform layer of a ceramic material, the layer being deposited by thermal decomposition of a non-alkoxylated organosilicon precursor in the vapor phase, in a steam containing gas atmosphere in order to form oxide ceramics.

Inventors

  • 👤 Terence Clark
  • 👤 Richard Cruse
  • 👤 Stephen Rohman
  • 👤 Robert Mininni

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 02:43
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/22; C23C16/30; C23C16/40; C23C16/401; C23C16/402

Claims Analysis

Total Claims: 36
Claim 1
Independent Claim 62 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor compound in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group.
Claim 2
Independent Claim 62 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor compound in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group.
Claim 3
Dependent Claim 18 words
The method of claim 1, wherein said precursor is an organosilicon compound containing nitrogen, carbon and hydrogen atoms.
Claim 4
Dependent Claim 27 words
The method of claim 2, wherein said precursor contains at least two silicon atoms, wherein at least two silicon atoms are bonded to a single nitrogen atom.
Claim 5
Dependent Claim 18 words
The method of claim 1, wherein said precursor is a silane having 1 to about 30 carbon atoms.
Claim 6
Dependent Claim 18 words
The method of claim 2, wherein said precursor is a silane having 1 to about 20 carbon atoms.
Claim 7
Dependent Claim 45 words
The method according to claim 1, wherein said ceramic material consists essentially of silicon, carbon, oxygen and nitrogen or silicon, carbon and oxygen, and said ceramic material contains 50 to 67 atomic % of oxygen and 0 to 30 atomic % of free elemental carbon.
Claim 8
Dependent Claim 25 words
The method according to claim 1, wherein said precursor is a silicon compound which is volatile at temperatures below those employed in the decomposition process.
Claim 9
Dependent Claim 89 words
The method of claim 1, wherein said precursor has the structure shown below ##STR7## wherein each R is, independently, hydrogen, C 1-20 alkyl, halogen or NR 1 R 2 , where R 1 and R 2 are hydrogen, C 1-20 alkyl or SiR 3 R 4 R 5 where R 3 , R 4 and R 5 are independently hydrogen, C 1-20 alkyl, halogen or NR 1 R 2 and X is H or SiR 3 R 4 R 5 with the proviso that the precursor is not hexamethyldisilazane.
Claim 10
Dependent Claim 33 words
The method of claim 8, wherein said precursor is selected from the group consisting of heptamethyl-chlorotrisilazane, 1,3-dichloro-1,1,3,3-tetramethyl disilazane, 1,2,3-trichloro hexamethyl trisilazane, ethyl-heptamethyl trisilazane, chloro-octamethyl trisilazane, nonamethyl trisilazane, 1,2,3-trichloro hexamethyl trisilazane, and 1,1-dichloro-1-ethyl-trimethyl disilazane.
Claim 11
Independent Claim 113 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group, and wherein said precursor has the structure shown below ##STR8## wherein each R 6 is independently hydrogen or C 1-20 alkyl, and each R 7 is independently hydrogen or SiR 8 R 9 R 10 , wherein R 8 , R 9 and R 10 are independently hydrogen or C 1-20 alkyl.
Claim 12
Independent Claim 113 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group, and wherein said precursor has the structure shown below ##STR8## wherein each R 6 is independently hydrogen or C 1-20 alkyl, and each R 7 is independently hydrogen or SiR 8 R 9 R 10 , wherein R 8 , R 9 and R 10 are independently hydrogen or C 1-20 alkyl.
Claim 13
Dependent Claim 20 words
The method of claim 10, wherein said precursor is selected from the group consisting of N-dimethylsilyl-1,1,3,3,5,5-hexamethyl-cyclotrisilazane; bis(N-dimethylsilyl)-1,1,3,3,5,5-hexamethyl-cyclotrisilazane; tris(N-dimethylsilyl)-1,1,3,3,5,5-hexamethylcyclotrisilazane; and 1,1,3,3,5,5-hexamethyltrisilazane.
Claim 14
Independent Claim 122 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group, and wherein said precursor has the structure shown below ##STR9## wherein each R 6 is independently hydrogen or C 1-20 alkyl, and each R 7 is independently hydrogen or SiR 8 R 9 R 10 , wherein R 8 , R 9 and R 10 are, independently, hydrogen or C 1-20 alkyl, and R 11 is hydrogen or C 1-20 alkyl.
Claim 15
Independent Claim 122 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group, and wherein said precursor has the structure shown below ##STR9## wherein each R 6 is independently hydrogen or C 1-20 alkyl, and each R 7 is independently hydrogen or SiR 8 R 9 R 10 , wherein R 8 , R 9 and R 10 are, independently, hydrogen or C 1-20 alkyl, and R 11 is hydrogen or C 1-20 alkyl.
Claim 16
Dependent Claim 19 words
The method of claim 10, wherein R 6 , R 7 and R 11 are independently C 1-8 alkyl.
Claim 17
Independent Claim 84 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group, and wherein said precursor has the structure shown below ##STR10## wherein R 6 and R 12 are independently hydrogen or C 1-20 alkyl.
Claim 18
Independent Claim 84 words
A method for passivating a surface of a chemical reactor subject to coking, comprising decomposing an organosilicon precursor in the vapor phase inside the reactor, in a steam-containing carrier gas atmosphere to form a thin layer of a ceramic material on the surface of the chemical reactor, wherein said precursor is an organosilicon compound which does not contain an alkoxy group, and wherein said precursor has the structure shown below ##STR10## wherein R 6 and R 12 are independently hydrogen or C 1-20 alkyl.
Claim 19
Dependent Claim 16 words
The method of claim 14, wherein R 6 and R 12 are independently C 1-8 alkyl.
Claim 20
Dependent Claim 82 words
The method of claim 1, wherein said precursor has the structure shown below ##STR11## wherein each R is independently hydrogen, C 1-20 alkyl, halogen or NR 1 R 2 , wherein R 1 and R 2 are independently hydrogen, C 1-20 alkyl, halogen or SiR 3 R 4 R 5 where R 3 , R 4 and R 5 are independently hydrogen, C 1-20 alkyl, halogen or NR 1 R 2 ; and A is a divalent alkylene, arylene or alkylarylene group.
Claim 21
Dependent Claim 29 words
The method of claim 16, wherein R, R 1 and R 2 are C 1-8 alkyl and A is C 2-6 alkylene, C 6-10 arylene or C 8-16 alkylarylene.
Claim 22
Dependent Claim 37 words
The method of claim 1, wherein said carrier gas is a mxiture of steam and a gas selected from the group consisting of nitrogen, argon, helium, methane, ethylene, ethane, hydrogen, carbon dioxide, carbon monoxide and mixtures thereof.
Claim 23
Dependent Claim 24 words
The method of claim 18, wherein the concentration of steam in said mixture is in the range between about 10 and 100 volume %.
Claim 24
Dependent Claim 11 words
The method of claim 1, wherein said carrier gas is steam.
Claim 25
Dependent Claim 16 words
The method of claim 19, wherein said carrier gas is a mixture of steam and nitrogen.
Claim 26
Dependent Claim 19 words
The method of claim 19, wherein said carrier gas is a mixture of steam, carbon monoxide and carbon dioxide.
Claim 27
Dependent Claim 21 words
The method of claim 1, wherein the concentration of said precursor in said carrier gas is less than 10.0 volume percent.
Claim 28
Dependent Claim 21 words
The method of claim 23, wherein the concentration of said precursor in said carrier gas is less than 5.0 volume percent.
Claim 29
Dependent Claim 22 words
The method of claim 4, wherein said process is thermal decomposition carried out at a temperature of between 600° and 1000° C.
Claim 30
Dependent Claim 14 words
The method of claim 25, wherein said temperature is between 700° and 900° C.
Claim 31
Dependent Claim 52 words
The method according to claim 2, wherein said precursor is selected from the group consisting of hexamethyldisilazane, tetramethylsilane, (diethylamino)trimethylsilane, nonamethyltrisilazane, (isopropylamino)trimethylsilane, (dimethylamino)trimethylsilane, heptamethyldisilazane, bis(isopropylamino)dimethylsilane, hexamethyldisilane, tetramethyldisilazane, (diethylamino)triethylsilane, tetrakis(dimethylamino)silane, bis(dimethylamino)methylsilane, (dimethylamino)triethylsilane, trimethylsilane, (dimethylamino)benzyldimethylsilane, (2-picolylamino)trimethylsilane, tris(dimethylamino)triethylsilane, tris(isopropylamino)methylsilane, dimethylsilane, bis(diethylamino)methylsilane, (dimethylamino)benzylmethylsilane, butylmethylphenylsilane, (diisopropylamino)methylchlorosilane, octamethyltrisilazane, bis(dimethylamino)phenylsilane, benzylmethylsilane, triisopropylsilane, tris(dimethylamino)methylsilane, diethylmethylsilane, triethylsilane, bis(dimethylamino) ethylsilane, hexamethyltrisilazane, and (dimethylamino)dimethylsilane.
Claim 32
Dependent Claim 24 words
The method of claim 1, wherein said precursor is selected from the group consisting of hexaethyldisiloxane, tris(trimethylsilylamino)ethylsiloxane, hexamethyldisiloxane, 1,1,3,3,5-hexamethylcyclotrisiloxane, tris(trimethylsilylamino)ethylsiloxane-mono-tetramethylsilane, tris(trimethylsilylamino)ethylsiloxane-di-tetramethylsilane, tris(trimethylsilylamino)ethylsiloxane-tri-tetramethylsilane, and octamethylcyclotetrasiloxane.
Claim 33
Dependent Claim 10 words
The method of claim 27, wherein said precursor is hexamethyldisilazane.
Claim 34
Dependent Claim 10 words
The method of claim 27, wherein said precursor is dimethylaminotriethylsilane.
Claim 35
Dependent Claim 10 words
The method of claim 27, wherein said precursor is tris(dimethylamino)triethylsilane.
Claim 36
Dependent Claim 45 words
The method of claim 2, wherein said precursor consists of a mixture of 30-10 volume % of at least one first compound selected from the group consisting of tris(dimethylamino)ethylsilane, bis(dimethylamino)diethylsilane, dimethylaminoethylsilane and tris(monomethylamino)ethylsilane, and 70-90 volume % of a precursor different than said first compound.

References Cited (Backward Citations)

US4099990A Cited
WO1990003452A1 Cited
US5208069A Cited

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