US4174228A
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Cementitious magnesia compositions containing salts of organo-silanols
Assignee: PPG Industries Inc
•
Filing: 1978-03-28
•
Granted: 1979-11-13
•
Expires: 1998-03-28
Abstract
Abstract Magnesium oxide cementitious compositions are disclosed containing salts of organo-silanols. The silanol salts are water-soluble and are characterized in having attached to the silicon atom at least one group comprising a moiety attached to the silicon atom through a substantially non-hydrolyzable silicon-carbon bond and at least one silanol group which is at least partially neutralized with a base. A magnesia composition containing one or more of these organo-silanol salts has improved casting, molding, or spraying properties, as compared to a magnesia composition lacking the silanol salt.
Inventors
- 👤 William G. Boberski
- 👤 Wen-Hsuan Chang
- 👤 Jerome A. Seiner
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 22:39
CPC Classifications
C; C04; C04B; C04B28/00; C04B28/30; C04B28/32; C04B24/00; C04B24/40; C04B24/42; C07; C07F; C07F7/00; C07F7/02; C07F7/08; C07F7/18; C07F7/1804
Claims Analysis
Total Claims: 69
Claim 1
Independent Claim
242 words
A moldable, castable or sprayable cementitious composition, comprising: (a) magnesium oxide; (b) a magnesium salt having at least moderate solubility in water; (c) at least one water-soluble organo-silanol salt, characterized in having attached to the silicon atom (i) at least one group comprising a water-soluble salt having the general formula: O.sup.- A.sup.+ where A + is a monovalent cation or one equivalent of a polyvalent cation and (ii) at least one group comprising an organo moiety attached to the silicon atom through a substantially non-hydrolyzable silicon-carbon bond with the organo moiety further characterized in having a working parameter of solubility, δ wp , in the range of about 6.2 to about 8.0 (cal./c.c.) 1/2 , with ##EQU3## wherein: F i =the molar attraction constant of an individual functional group of said moiety expressed in (cal. c.c.) 1/2 per mole, and V i =the molar volume constant of an individual group of said moiety expressed in c.c. per mole; and (d) a liquid phase comprising water; wherein the mole ratio of the magnesium oxide to the magnesium salt ranges from 3:1 to 10:1, the level or organo-silanol salt ranges from about 0.5 percent to about 10 percent by weight of the magnesium oxide and the level of water is in an amount effective to cause reaction of at least a portion of said magnesium oxide and at least a portion of said magnesium salt to form a matrix curable to a hardened state.
Claim 2
Dependent Claim
242 words
A moldable, castable or sprayable cementitious composition, comprising: (a) magnesium oxide; (b) a magnesium salt having at least moderate solubility in water; (c) at least one water-soluble organo-silanol salt, characterized in having attached to the silicon atom (i) at least one group comprising a water-soluble salt having the general formula: O.sup.- A.sup.+ where A + is a monovalent cation or one equivalent of a polyvalent cation and (ii) at least one group comprising an organo moiety attached to the silicon atom through a substantially non-hydrolyzable silicon-carbon bond with the organo moiety further characterized in having a working parameter of solubility, δ wp , in the range of about 6.2 to about 8.0 (cal./c.c.) 1/2 , with ##EQU3## wherein: F i =the molar attraction constant of an individual functional group of said moiety expressed in (cal. c.c.) 1/2 per mole, and V i =the molar volume constant of an individual group of said moiety expressed in c.c. per mole; and (d) a liquid phase comprising water; wherein the mole ratio of the magnesium oxide to the magnesium salt ranges from 3:1 to 10:1, the level or organo-silanol salt ranges from about 0.5 percent to about 10 percent by weight of the magnesium oxide and the level of water is in an amount effective to cause reaction of at least a portion of said magnesium oxide and at least a portion of said magnesium salt to form a matrix curable to a hardened state.
Claim 3
Dependent Claim
39 words
The cementitious composition of claim 1, wherein said magnesium salt is selected from the group consisting of magnesium chloride, hydrated magnesium chloride, magnesium sulphate, hydrated magnesium sulphate, hydrated magnesium nitrate, hydrated magnesium acetate, magnesium bromide and hydrated magnesium bromide.
Claim 4
Dependent Claim
27 words
The cementitious composition of claim 1, wherein said monovalent cation is selected from the group consisting of tertiary sulphonium, ammonium, substituted ammonium, quaternary ammonium and quaternary phosphonium.
Claim 5
Dependent Claim
22 words
The cementitious composition of claim 1, wherein said monovalent cation is selected from the group consisting of Group IA alkali metal cations.
Claim 6
Dependent Claim
63 words
The cementitious composition of claim 1, wherein said organo-silanol is a hydrolyzate of an organo-silicon compound, said organo-silicon compound characterized in having attached to its silicon atom one or two groups having a hydrolyzable bond with the silicon atom and selected from the group consisting of alkoxyl, aryloxyl, substituted aryloxyl, aralkoxy, substituted aralkoxyl, alylamino, substituted alkylamino, silylamino, substituted silylamino, mercapto and substituted mercapto.
Claim 7
Dependent Claim
49 words
The cementitious composition of claims 1 or 5, wherein said organo moiety comprises alkyl or oxalkyl group which may be substituted with one or more groups selected from the group consisting of alkyl, alkoxy, aryl, aryloxy, substituted aryloxy, acrylyl, substituted acrylyl, carboxy, carboalkoxy, amino, amido, ureido, oxiranyl and sulphur.
Claim 8
Dependent Claim
40 words
The cementitious composition of claim 5, wherein said organo-silicon compound is a reaction product of a compound containing acrylyl or substituted acrylyl groups and a silane having an organo moiety comprising an amino group containing at least one active hydrogen.
Claim 9
Dependent Claim
36 words
The cementitious composition of claim 5, wherein said organo-silicon compound is a reaction product of an amino-compound having at least one active hydrogen and a silane having an organo moiety comprising acrylyl or substituted acrylyl groups.
Claim 10
Dependent Claim
54 words
The cementitious composition of claim 5, wherein said organo-silicon compound is a reaction product of an silane having an organo moiety containing an epoxy group and a compound containing a chemical group selected from the group consisting of amino, amide, ureido, urea, urethane, thiol and hydroxyl, each having at least one active hydrogen atom.
Claim 11
Dependent Claim
54 words
The cementitious composition of claim 5, wherein said organo-silicon compound is a reaction product of an epoxy-containing compound and a silane having an organo moiety comprising one or more chemical groups selected from the group consisting of primary amino, secondary amino, amide, urea, urethane and thiol, each having at least one active hydrogen atom.
Claim 12
Dependent Claim
20 words
The cementitious composition of claim 10, wherein said epoxycontaining compound is an aliphatic epoxide and said silane is an aminoalkylsilane.
Claim 13
Dependent Claim
18 words
The cementitious composition of claim 11, wherein said aliphatic epoxide is 1,2-butylene oxide and said aminoalkylsilane is γ-aminopropyltriethoxysilane.
Claim 14
Dependent Claim
18 words
The cementitious composition of claim 11, wherein said aliphatic epoxide is 1,2-butylene oxide and said aminoalkylsilane is N-β-aminoethyl-γ-aminopropyltrimethoxysilane.
Claim 15
Dependent Claim
18 words
The cementitious composition of claim 10, wherein said epoxy-containing compound is 1,2-butylene oxide and said silane is ureidopropyltriethoxysilane.
Claim 16
Dependent Claim
21 words
The cementitious composition of claim 10, wherein said epoxy-containing compound is an aliphatic epoxide and said silane is a thioalkyl silane.
Claim 17
Dependent Claim
19 words
The cementitious composition of claim 15, wherein said aliphatic epoxide is 1,2-butylene oxide and said thioalkyl silane is mercaptoethyltriethoxysilane.
Claim 18
Dependent Claim
20 words
The cementitious composition of claim 10, wherein said epoxy-containing compound is an aliphatic polyepoxide and said silane is an aminoalkylsilane.
Claim 19
Dependent Claim
19 words
The cementitious composition of claim 17, wherein said aliphatic polyepoxide is 1,4-butanediol di-glycidyl ether and said aminoalkylsilane is γ-aminopropyltriethoxysilane.
Claim 20
Dependent Claim
14 words
The cementitious composition of claim 5, wherein said organo-silicon compound has the structure: ##STR29##
Claim 21
Dependent Claim
14 words
The cementitious composition of claim 5, wherein said organo-silicon compound has the structure: ##STR30##
Claim 22
Dependent Claim
14 words
The cementitious composition of claim 5, wherein said organo-silicon compound has the structure: ##STR31##
Claim 23
Dependent Claim
14 words
The cementitious composition of claim 5, wherein said organo-silicon compound has the structure: ##STR32##
Claim 24
Dependent Claim
14 words
The cementitious composition of claim 1, wherein said organo-silanol salt has the structure: ##STR33##
Claim 25
Dependent Claim
14 words
The cementitious composition of claim 1, wherein said organo-silanol salt has the structure: ##STR34##
Claim 26
Dependent Claim
24 words
The cementitious composition of claim 1 further comprising a material selected from the group consisting of fibrous glass, sisal, mica, mineral wool and cotton.
Claim 27
Dependent Claim
26 words
The cementitious composition of claim 1 further comprising a thickening agent selected from the group consisting of hydroxyethyl cellulose, hydroxypropyl cellulose, polyethylene oxide and polyvinyl alcohol.
Claim 28
Dependent Claim
46 words
The cementitious composition of claim 1 wherein the mole ratio of magnesium oxide to the magnesium salt ranges from 6:1 to 7.5:1 and the level of organo-silanol salt in the composition ranges from about 2 percent to about 5 percent by weight of the magnesium oxide.
Claim 29
Dependent Claim
260 words
A process for forming an article from a curable cementitious composition, comprising: (a) mixing together in the presence of a liquid phase having water sufficient to produce a moldable, curable slurry composition, the components of: (1) magnesium oxide; (2) at least one magnesium salt having moderate solubility in water; and (3) at least one water-soluble organo-silanol salt, characterized in having attached to the silicon atom (i) at least one group comprising a water-soluble salt having the general formula: O-A.sup.+ where A + is a monovalent cation or one equivalent of a polyvalent cation and (ii) at least one group comprising an organo moiety attached to the silicon atom through a substantially non-hydrolyzable silicon-carbon bond with the organo moiety further characterized in having a working parameter of solubility, δ wp , in the range of about 6.2 to about 8.0 (cal.c.c.) 1/2 , with ##EQU4## wherein: F i =the molar attraction constant of an individual functional group of said moiety expressed in (cal.c.c.) 1/2 per mole, and V i =the molar volume constant of an individual group of said moiety expressed in c.c. per mole; and wherein the mole ratio of the magnesium oxide to the magnesium salt ranges from 3:1 to 10:1, the level of organo-silanol salt ranges from about 0.5 percent to about 10 percent by weight of the magnesium oxide (b) placing said slurry composition in a mold form; and (c) allowing said composition to cure sufficiently such that said article may be removed from the mold form without substantially adversely affecting the integrity of the molded article.
Claim 30
Dependent Claim
260 words
A process for forming an article from a curable cementitious composition, comprising: (a) mixing together in the presence of a liquid phase having water sufficient to produce a moldable, curable slurry composition, the components of: (1) magnesium oxide; (2) at least one magnesium salt having moderate solubility in water; and (3) at least one water-soluble organo-silanol salt, characterized in having attached to the silicon atom (i) at least one group comprising a water-soluble salt having the general formula: O-A.sup.+ where A + is a monovalent cation or one equivalent of a polyvalent cation and (ii) at least one group comprising an organo moiety attached to the silicon atom through a substantially non-hydrolyzable silicon-carbon bond with the organo moiety further characterized in having a working parameter of solubility, δ wp , in the range of about 6.2 to about 8.0 (cal.c.c.) 1/2 , with ##EQU4## wherein: F i =the molar attraction constant of an individual functional group of said moiety expressed in (cal.c.c.) 1/2 per mole, and V i =the molar volume constant of an individual group of said moiety expressed in c.c. per mole; and wherein the mole ratio of the magnesium oxide to the magnesium salt ranges from 3:1 to 10:1, the level of organo-silanol salt ranges from about 0.5 percent to about 10 percent by weight of the magnesium oxide (b) placing said slurry composition in a mold form; and (c) allowing said composition to cure sufficiently such that said article may be removed from the mold form without substantially adversely affecting the integrity of the molded article.
Claim 31
Dependent Claim
41 words
The process of claim 28, wherein said components are mixed together by (a) firstly, preparing a blend of said magnesium oxide and said organo-silanol salt; and (b) subsequently mixing said blend with said magnesium salt in the presence of said water.
Claim 32
Dependent Claim
29 words
The process of claim 28 further comprising introducing into said slurry composition a material selected from the group consisting of fibrous glass, sisal, silicas, mica, mineral wool and cotton.
Claim 33
Dependent Claim
20 words
The process of claim 28 further comprising forming said article with the aid of compression force of heat, or both.
Claim 34
Dependent Claim
38 words
The process of claim 28, wherein said magnesium salt is selected from the group consisting of mangesium chloride, hydrated magnesium chloride, magnesium sulphate, hydrated magnesium sulphate, hydrated magnesium nitrate, hydrated magnesium acetate, magnesium bromide and hydrated magnesium bromide.
Claim 35
Dependent Claim
31 words
The process of claim 28, wherein said monovalent cation is selected from the group consisting of tertiary sulphonium, ammonium, substituted ammonium, quaternary ammonium, quaternary phosphonium and Group IA alkali metal cations.
Claim 36
Dependent Claim
48 words
The process of claim 28, wherein said organo moiety of said organo-silanol comprises alkyl group which may be substituted with one or more groups selected from the group consisting of alkyl or alkoxyl groups of one to about eight carbon atoms, primary amino group and secondary amino group.
Claim 37
Dependent Claim
62 words
The process of claim 28, wherein said organosilanol is a hydrolyzate of an organo-silicon compound, said organo-silicon compound characterized in having attached to its silicon atom one or two groups having a hydrolyzable bond with the silicon atom and selected from the group consisting of alkoxyl, aryloxyl, substituted aryloxyl, aralkoxyl, substituted aralkoxyl, alkylamino, substituted alkylamino, silylamino, substituted silylamino, mercapto and substituted mercapto.
Claim 38
Dependent Claim
48 words
The process of claims 28 or 35 wherein said organo moiety comprises alkyl or oxalkyl group which may be substituted with one or more groups selected from the group consisting of alkyl, alkoxy, aryl, aryloxy, substituted aryloxy, acrylyl, substituted acrylyl, carboxy, carboalkoxy, amino, amido, ureido, oxiranyl and sulphur.
Claim 39
Dependent Claim
39 words
The process of claim 35, wherein said organo-silicon compound is a reaction product of a compound containing acrylyl or substituted acrylyl groups and a silane having an organo moiety comprising an amino group containing at least one active hydrogen.
Claim 40
Dependent Claim
35 words
The process of claim 35, wherein said organo-silicon compound is a reaction product of an amino-compound having at least one active hydrogen and a silane having an organo moiety comprising acrylyl or substituted acrylyl groups.
Claim 41
Dependent Claim
52 words
The process of claim 35, wherein said organo-silicon compound is a reaction product of a silane having an organo moiety containing an epoxy group and a compound containing a chemical group selected from the group consisting of amino, amide, ureido, urea, urethane, thiol and hydroxyl, each having at least one active hydrogen.
Claim 42
Dependent Claim
53 words
The process of claim 35, wherein said organo-silicon compound is a reaction product of an epoxy-containing compound and a silane having an organo moiety comprising one or more chemical groups selected from the group consisting of primary amino, secondary amino, amide, urea, urethane and thiol, each having at least one active hydrogen atom.
Claim 43
Dependent Claim
19 words
The process of claim 40, wherein said epoxy-containing compound is an aliphatic epoxide and said silane is an aminoalkylsilane.
Claim 44
Dependent Claim
22 words
The process of claim 35, wherein said organo-silicon compound is selected from the group consisting of compounds illustrated by the formulae: ##STR35##
Claim 45
Dependent Claim
54 words
The process of claim 35, wherein said organo-silicon compound is seleced from the group consisting of (a) a reaction product of 1,2-butylene oxide and γ-aminopropyltriethoxysilane; (b) a reaction product of 1,2-butylene oxide and ureidopropyltriethoxysilane; (c) a reaction product of 1,2-butylene oxide and mercaptoethyltriethoxysilane; and (d) a reaction product of 1,4-butanediol diglycidyl ether and γ-aminopropyltriethoxysilane.
Claim 46
Dependent Claim
13 words
The process of claim 28, wherein said organo-silanol salt has the structure: ##STR36##
Claim 47
Dependent Claim
13 words
The process of claim 28, wherein said organo-silanol salt has the structure: ##STR37##
Claim 48
Dependent Claim
43 words
The process of claim 28 wherein the level of the magnesium oxide to the magnesium salt ranges from 6:1 to 7.5:1 and the level of the organo-silanol salt ranges from about 2 percent to about 5 percent by weight of the magnesium oxide.
Claim 49
Dependent Claim
9 words
A product produced by the process of claim 28.
Claim 50
Dependent Claim
248 words
A storage stable two-package system for forming in the presence of water a moldable, castable or sprayable cementitious material when a first composition is mixed with a second composition, comprising: (a) said first composition including at least one magnesium salt having at least moderate solubility in water; and (b) said second composition prepared from mixing together (1) magnesium oxide; and (2) at least one water-soluble organo-silanol salt, characterized in having attached to the silicon atom (i) at least one group comprising a water-soluble salt having the general formula: O.sup.- A.sup.+ where A + is a monovalent cation or one equivalent of a polyvalent cation and (ii) at least one group comprising an organo moiety attached to the silicon atom through a substantially nonhydrolyzable silicon-carbon bond with the organo moiety further characterized in having a working parameter of solubility, δ wp , in the range of about 6.2 to about 8.0 (cal./c.c.) 1/2 , with ##EQU5## wherein: F i =the molar attraction constant of an individual functional group of said moiety expressed in (cal. c.c.) 1/2 per mole, and V i =the molar volume constant of an individual group of said moiety expressed in c.c. per mole; with the organo-silicon compound at a level ranging from about 0.5 percent to about 10 percent by weight of the magnesium oxide; said compositions being mixed at time of use at levels to provide a mole ratio of the magnesium oxide to the magnesium salt of from about 3:1 to about 10:1.
Claim 51
Dependent Claim
248 words
A storage stable two-package system for forming in the presence of water a moldable, castable or sprayable cementitious material when a first composition is mixed with a second composition, comprising: (a) said first composition including at least one magnesium salt having at least moderate solubility in water; and (b) said second composition prepared from mixing together (1) magnesium oxide; and (2) at least one water-soluble organo-silanol salt, characterized in having attached to the silicon atom (i) at least one group comprising a water-soluble salt having the general formula: O.sup.- A.sup.+ where A + is a monovalent cation or one equivalent of a polyvalent cation and (ii) at least one group comprising an organo moiety attached to the silicon atom through a substantially nonhydrolyzable silicon-carbon bond with the organo moiety further characterized in having a working parameter of solubility, δ wp , in the range of about 6.2 to about 8.0 (cal./c.c.) 1/2 , with ##EQU5## wherein: F i =the molar attraction constant of an individual functional group of said moiety expressed in (cal. c.c.) 1/2 per mole, and V i =the molar volume constant of an individual group of said moiety expressed in c.c. per mole; with the organo-silicon compound at a level ranging from about 0.5 percent to about 10 percent by weight of the magnesium oxide; said compositions being mixed at time of use at levels to provide a mole ratio of the magnesium oxide to the magnesium salt of from about 3:1 to about 10:1.
Claim 52
Dependent Claim
29 words
The two-package system of claim 48, wherein said first composition further comprises water in an amount effective to form a saturated or nearly saturated solution with said magnesium salt.
Claim 53
Dependent Claim
39 words
The two-package system of claim 48, wherein said magnesium salt is selected from the group consisting of magnesium chloride, hydrated magnesium chloride, magnesium sulphate, hydrated magnesium sulphate, hydrated magnesium nitrate, hydrated magnesium acetate, magnesium bromide and hydrated magnesium bromide.
Claim 54
Dependent Claim
32 words
The two-package system of claim 48, wherein said monovalent cation is selected from the group consisting of tertiary sulphonium, ammonium, substituted ammonium, quaternary ammonium, quaternary phosphonium and Group IA alkali metal cations.
Claim 55
Dependent Claim
41 words
The two-package system of claim 48, wherein said organo moiety comprises alkyl group which may be substituted with one or more groups selected from the group consisting of alkyl of one to about eight carbon atoms, primary amino and secondary amino.
Claim 56
Dependent Claim
63 words
The two-package system of claim 48, wherein said organo-silanol is a hydrolyzate of an organo-silicon compound, said organo-silicon compound characterized in having attached to its silicon atom one or two groups having a hydrolyzable bond with the silicon atom and selected from the group consisting of alkoxyl, aryloxyl, substituted aryloxyl, aralkoxyl, substituted aralkoxyl, alkylamino, substituted alkylamino, silylamino, substituted silylamino, mercapto and substituted mercapto.
Claim 57
Dependent Claim
49 words
The two-package system of claims 48 or 53, wherein said organo moiety comprises alkyl or oxalkyl group which may be substituted with one or more groups selected from the group consisting of alkyl, alkoxy, aryl, aryloxy, substituted aryloxy, acrylyl, substituted acrylyl, carboxy, carboalkoxy, amino, amido, ureido, epoxy and sulphur.
Claim 58
Dependent Claim
40 words
The two-package system of claim 53, wherein said organo-silicon compound is a reaction product of a compound containing acrylyl or substituted acrylyl groups and a silane having an organo moiety comprising an amino group containing at least one active hydrogen.
Claim 59
Dependent Claim
36 words
The two-package system of claim 53, wherein said organo-silicon compound is a reaction product of an amino-compound having at least one active hydrogen and a silane having an organo moiety comprising acrylyl or substituted acrylyl groups.
Claim 60
Dependent Claim
54 words
The two-package system of claim 53, wherein said organo-silicon compound is a reaction product of a silane having an organo moiety containing an epoxy group and a compound containing a chemical group selected from the group consisting of amino, amide, ureido, urea, urethane, thiol and hydroxyl, each having at least one active hydrogen atom.
Claim 61
Dependent Claim
54 words
The two-package system of claim 53, wherein said organo-silicon compound is a reaction product of an epoxy-containing compound and a silane having an organo moiety comprising one or more chemical groups selected from the group consisting of primary amino, secondary amino, amide, urea, urethane and thiol, each having at least one active hydrogen atom.
Claim 62
Dependent Claim
20 words
The two-package system of claim 58, wherein said epoxy-containing compound is an aliphatic epoxide and said silane is an aminoalkylsilane.
Claim 63
Dependent Claim
23 words
The two-package system of claim 53, wherein said organo-silicon compound is selected from the group consisting of compounds illustrated by the formulae: ##STR38##
Claim 64
Dependent Claim
55 words
The two-package system of claim 53, wherein said organo-silicon compound is selected from the group consisting of (a) a reaction product of 1,2-butylene oxide and γ-aminopropyltriethoxysilane; (b) a reaction product of 1,2-butylene oxide and ureidopropyltriethoxysilane; (c) a reaction product of 1,2-butylene oxide and mercaptoethyltriethoxysilane; and (d) a reaction product of 1,4-butanediol diglycidyl ether and γ-aminopropyltriethoxysilane.
Claim 65
Dependent Claim
14 words
The two-package system of claim 48, wherein said organosilanol salt has the structure: ##STR39##
Claim 66
Dependent Claim
14 words
The two-package system of claim 48, wherein said organosilanol salt has the structure: ##STR40##
Claim 67
Dependent Claim
32 words
The two-package system of claim 48, wherein at least one of said compositions further comprises a material selected from the group consisting of fibrous glass, sisal, silica, mica, mineral wool and cotton.
Claim 68
Dependent Claim
33 words
The two-package system of claim 48, wherein at least one of said compositions further comprises a thickening agent selected from the group consisting of hydroxyethyl cellulose, hydroxypropyl cellulose, polyethylene oxide and polyvinyl alcohol.
Claim 69
Dependent Claim
28 words
The two-package system of claim 48 wherein the level of the organo-silanol salt ranges from about 2 percent to about 5 percent by weight of the magnesium oxide.
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) | 1982-11-12 | 1983-05-14 | 1983-11-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-11-12 | 1987-05-14 | 1987-11-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-11-12 | 1991-05-14 | 1991-11-13 | $7700.00 | Window Closed / Lapsed |