Patent EP0767216A1 successfully refreshed from Google Patents.
EP0767216A1
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High strength silicone resin/fluid alloy compositions and method of making
Assignee: Dow Silicones Corp
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Filing: 1996-09-11
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Granted: —
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Expires: 2016-09-11
Abstract
Abstract Silicone resin/fluid alloy compositions that exhibit high strength and toughness over a predetermined service temperature range are prepared by blending functional resins and fluids and then cross-linking in a manner such that unusually high ultimate tensile strengths, shear loss moduli and loss tangents are obtained. The desirable mechanical properties are dependent upon the number average molecular weights of the resin and fluid, the ratio of resin/fluid and control of the cross-link density between the resin and fluid.
Inventors
- 👤 Randall Gene Schmidt
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-11-09 23:09
CPC Classifications
C; C08; C08L; C08L83/00; C08L83/04; C08G; C08G77/00; C08G77/04; C08G77/12; C08G77/14; C08G77/16; C08G77/18; C08G77/20; C08G77/22; C08G77/26; C08G77/70
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
472 words
A method of making a silicone resin/fluid alloy that exhibits high strength and toughness over a predetermined service temperature range having a lower limit of not less than -120°C. and an upper limit not greater than 250°C., said method comprising the steps of: (I) blending, to substantial homogeneity, (A) an organosilicone resin of the empirical formula [R 3 SiO 1/2 ] a [R 2 SiO 2/2 ] b [RSiO 3/2 ] c [SiO 4/2 ] d wherein: a, b, c and d are positive numerical values with the provisos that a + b + c + d = 1 , 1/2(b + c + d) ≤ a ≤ (b + c + d) and 0 ≤ (b + c)/d ≤ 0.2; R is a monovalent radical independently selected from the group consisting of hydrogen, hydroxyl, alkyl, alkenyl, alkoxy, oximo, aryl, epoxide, carboxyl, ether, amide and alkyl amino radicals, which R groups may be the same or different, with the proviso that at least sixty mole percent of said R radicals are methyl; the organosilicone resin (A) has a number average molecular weight (Mn) between 2,000 and 7,000; and (B) a predominantly linear silicone fluid having the empirical formula [R' 3 SiO 1/2 ] x [R' 2 SiO 2/2 ] y [R'SiO 3/2 ] z wherein: x, y and z are positive numerical values with the provisos that x + y + z = 1 and y/(x + y + z) ≥ 0.9 ; and R' is a monovalent radical independently selected from the group consisting of hydrogen, hydroxyl, alkyl, alkenyl, alkoxy, oximo, aryl, epoxide, carboxyl, ether, amide and alkyl amino radicals, which R' groups may be the same or different, with the proviso that at least ninety mole percent of said R' radicals are methyl; said organosilicon resin (A) being present in an amount of 45 to 80 parts by weight and said predominantly linear silicone fluid (B) being present in an amount of 55 to 20 parts by weight, per 100 parts, by weight of the combined total of (A) and (B); (II) cross-linking the substantially homogeneous blend of (A) and (B) produced in step (I) with a cross-linker (C); said cross-linker having at least three functional groups associated therewith, which functional groups render said cross-linker copolymerizable with said organosilicone resin (A) and said predominantly linear silicone fluid (B); said cross-linking step being carried out to a predetermined cross-link density such that the cross-linked product of (A) and (B), when free of an inorganic filler, exhibits the following mechanical properties over the predetermined service temperature range: an ultimate tensile strength greater than or equal to 2.75 x 10 6 Pa (400 psi); a shear loss modulus G'' greater than or equal to 10 6 Newtons per m 2 ; and a loss tangent (tan δ) greater than or equal to 0.10.
Claim 2
Dependent Claim
61 words
A method in accordance with claim 1 wherein a predetermined number average of said R radicals per molecule (rRn) of said organosilicone resin (A) are reactive with said functional groups of said cross-linker (C) so as to render said organosilicone resin (A) copolymerizable with said cross-linker (C) and said predetermined number average of R groups limits the predetermined the cross-link density.
Claim 3
Dependent Claim
62 words
A method in accordance with claim 1 wherein a predetermined number average of said R' radicals per molecule (rR'n) of said predominantly linear silicone fluid (B) are reactive with said functional groups of said cross-linker (C) so as to render said fluid (B)) copolymerizable with said cross-linker (C) and said predetermined number average of R' groups limits the predetermined the cross-link density.
Claim 4
Dependent Claim
26 words
A method in accordance with claim 1 wherein said cross-linking step is carried out to said predetermined cross-link density by limiting the amount of cross-linker used.
Claim 5
Dependent Claim
520 words
A silicone resin/fluid alloy composition that exhibits high strength and toughness over a predetermined service temperature range having a lower limit of not less than -120°C. and an upper limit not greater than 250°C., said silicone resin/fluid alloy composition comprising: (A) an organosilicone resin of the empirical formula [R 3 SiO 1/2 ] a [R 2 SiO 2/2 ] b [RSiO 3/2 ] c [SiO 4/2 ] d wherein: a, b, c and d are positive numerical values with the provisos that a + b + c + d = 1 , 1/2(b + c + d) ≤ a ≤ (b + c + d) and 0 ≤ (b + c)/d ≤ 0.2; R is a monovalent radical independently selected from the group consisting of hydrogen, hydroxyl, alkyl, alkenyl, alkoxy, oximo, aryl, epoxide, carboxyl, ether, amide and alkyl amino radicals, which R groups may be the same or different, with the proviso that at least sixty mole percent of said R radicals are methyl; and the organosilicone resin (A) has a number average molecular weight (Mn) between 2,000 and 7,000; and (B) a predominantly linear silicone fluid having the empirical formula [R' 3 SiO 1/2 ] x [R' 2 SiO 2/2 ] y [R'SiO 3/2 ] z wherein: x, y and z are positive numerical values with the provisos that x + y + z = 1 and y/(x + y + z) ≥ 0:9 ; and R' is a monovalent radical independently selected from the group consisting of hydrogen, hydroxyl, alkyl, alkenyl, alkoxy, oximo, aryl, epoxide, carboxyl, ether, amide and alkyl amino radicals, which R' groups may be the same or different, with the proviso that at least ninety mole percent of said R' radicals are methyl; said organosilicon resin (A) being present in an amount of 45 to 80 parts by weight and said predominantly linear silicone fluid (B) being present in an amount of 55 to 20 parts by weight, per 100 parts, by weight of the combined total of (A) and (B); (C) a predetermined quantity of a cross-linker having at least three functional groups per molecule; a predetermined number average of said R radicals per molecule (rRn) of said organosilicone resin (A) being reactive with said functional groups of said cross-linker (C) so as to render said organosilicone resin (A) copolymerizable with said cross-linker (C); a predetermined number average of said R' radicals per molecule (rR'n) of said predominantly linear silicone fluid (B) being reactive with said functional groups of the cross-linker (C) so as to render the predominantly linear silicone fluid (B) copolymerizable with the cross-linker (C); and the respective predetermined number averages rRn and rR'n and the predetermined quantity of the cross-linker being selected such that: the silicone polymer alloy composition, when cross-linked and free of an inorganic filler, exhibits the following mechanical properties over the predetermined service temperature range: an ultimate tensile strength greater than or equal to 2.75 x 10 6 Pa; a shear loss modulus G'' greater than or equal to 10 6 Newtons per m 2 ; and a loss tangent, tan (δ) greater than or equal to 0.10.
Claim 6
Dependent Claim
15 words
A composition in accordance with claim 5 wherein rRn is between 1 and 6, inclusive.
Claim 7
Dependent Claim
13 words
A composition in accordance with claim 5 wherein rR'n is at least 2.
Claim 8
Dependent Claim
54 words
A composition in accordance with claim 7 wherein the number average of [R' 2 SiO 2/2 ] units between said at least two R' that are reactive with said functional groups of said cross-linker (C) defines a nonfunctional linear chain length and said number average nonfunctional linear chain length is between 100 and 10,000.
Claim 9
Dependent Claim
34 words
A composition in accordance with claim 8 wherein rRn is between 1 and 2.5 and said number average nonfunctional linear chain length of said predominantly linear silicone fluid (B) is between 100 and 400.
Claim 10
Dependent Claim
34 words
A composition in accordance with claim 8 wherein rRn is between 2.5 and 4 and said number average nonfunctional linear chain length of said predominantly linear silicone fluid (B) is between 400 and 2,500.
Claim 11
Dependent Claim
37 words
A composition in accordance with claim 5 further comprising a catalyst (D), said catalyst being provided in an amount sufficient to cause accelerated copolymerization between said organosilicone resin (A), said silicone fluid (B) and said cross-linker (C).
Claim 12
Dependent Claim
77 words
A composition in accordance with claim 11 further comprising: a platinum catalyst (D); said at least three functional groups of said cross-linker (C) being silicon-bonded hydrogen; said R radicals of said organosilicone resin (A) that are reactive with said at least three functional groups of said cross-linker (C) being vinyl radicals; and said R' radicals of said silicone fluid (B) that are reactive with said at least three functional groups of said cross-linker (C) being vinyl radicals.
Claim 13
Dependent Claim
13 words
A composition in accordance with claim 12 further comprising a catalyst inhibitor (E).
Claim 14
Dependent Claim
19 words
A composition in accordance with claim 5 further exhibiting optical clarity characterized by a reflectance of 2% or less.
Claim 15
Dependent Claim
38 words
A composition in accordance with claim 5 wherein said cross-linker is provided in an amount less than that required for stoichiometric reaction between the functional groups thereof and said R groups and R' groups that are reactive therewith.
References Cited (Backward Citations)
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