Claims
- 1. A process for the preparation of a stable silicone oil containing ≡SiH groups, starting with reagents which are a first silicone oil containing ≡SiH groups and monomers, this process comprising the steps of:(a) adding in a reactor an amount of from 5 to 5000 ppm, of heterogeneous catalytic composition relative to the total mass of the reagents; (b) adding said first silicone oil in said reactor; (c) heating to a temperature of between 25° C. and 200° C.; then (d) adding the monomers over a period of time of between 0 and 24 hour in said reactor, the monomer/≡SiH molar ratio of said oil being between 0.0001 and 1; then (e) separating the silicone oil obtained containing ≡SiH groups from the heterogeneous catalytic composition; and (f) finally devolatilizing the silicone oil containing ≡SiH groups to obtain the stable silicone oil; said monomers having the formula: wherein:the symbols R1 and R2, being identical or different, are a hydrogen atom, a phenyl radical or a linear or branched alkyl radical containing from 1 to 12 carbon atoms; the symbol Y corresponds to Y′-Y″-Y′ wherein: the symbol Y″ is a divalent radical selected from the group consisting of: —(C═O)—, —(NH)—, —O—, —(C═O)—O—, —NH—(C═O)—, and a free valency, the symbols Y′, being identical or different, is a divalent hydrocarbon-radical selected from the group consisting of linear alkyl radicals containing from 1 to 6 carbon atoms, branched alkyl radicals containing from 1 to 6 carbon atoms, and a free valency, optionally one of the radicals Y′ being a phenyl radical or an alkylaryl radical wherein the linear or branched alkyl part of the alkylaryl radical comprises 1 to 6 carbon atoms. wherein:the symbol Z is a monovalent radical —NHR4 or OH, the symbols R3 and R4, being identical or different, are a hydrogen atom, a phenyl radical or a linear or branched alkyl radical containing from 1 to 12 carbon atoms; the symbol Y corresponds to Y′-Y″-Y′, wherein: the symbol Y″ is a divalent radical selected from the group consisting of: —(C═O)—, —(NH)—, —O—, —(C═O)—O—, —NH—(C═O)— and a free valency, the symbols Y′, being identical or different, are a divalent hydrocarbon-based radical selected from the group consisting of linear alkyl radicals containing from 1 to 6 carbon atoms, branched alkyl radicals containing from 1 to 6 carbon atoms, and a free valency, optionally one of the radicals Y′ being a phenyl radical or an alkylaryl radical wherein the linear or branched alkyl part of the alkylaryl radical comprises 1 to 6 carbon atoms, in which:the symbol U is a divalent radical selected from the group consisting of: —NH—, —(C═O)—, —(C═O)—NH—, and —(C═O)—O—(C═O)—, the symbol R5 is a hydrogen atom, a phenyl radical and linear or branched alkyl radicals containing from 1 to 12 carbon atoms; the symbols W1 and W2, being identical or different, is a divalent hydrocarbon-based radical selected from the group consisting of a phenyl radical, linear alkyl radicals containing from 1 to 12 carbon atoms, branched alkyl radicals containing from 1 to 12 carbon atoms, alkylaryl radicals wherein the linear or branched alkyl part of the alkylaryl radical comprises 1 to 6 carbon atoms, and a free valency, the symbol Y corresponds to Y′-Y″-Y′, wherein: the symbol Y″ is a divalent radical selected from the group consisting of: —(C═O)—, —(NH)—, —O—, —(C═O)—O—, —NH—(C═O)—, and a free valency. the symbols Y′, being identical or different, is a divalent hydrocarbon-based radical selected from the group consisting of linear alkyl radicals containing from 1 to 6 carbon atoms, branched alkyl radicals containing from 1 to 6 carbon atoms, and a free valency, optionally one of the radicals Y′ being a phenyl radical or an alkylaryl radical wherein the linear or branched alkyl part comprises 1 to 6 carbon atoms,
- 2. A process according to claim 1, wherein:in step (a) the amount of heterogeneous catalytic composition is from 10 to 100 ppm relative to the total mass of the reagents; in step (c) said reaction medium is heated to a temperature of between 50° C. and 160° C.; and in step (d) the period of time of adding the monomers is between 2.5 and 5 h.
- 3. A process according to claim 1, wherein in step (e) the separation of the silicone is carried out by filtration.
- 4. A process according to claim 1, wherein said monomers bear a vinyl or allylic unit.
- 5. A process according claim 1, wherein R1, R2, R3, R4, and R5 identical or different are a hydrogen atom or a methyl radical.
- 6. A process according to claim 1, wherein the heterogeneous catalytic composition comprises a metal selected from the group consisting of cobalt, rhodium, ruthenium, platinum and nickel, deposited on an inert support.
- 7. A process according to claim 6, wherein the metal is platinum.
- 8. A process according to claim 6, wherein the inert support is selected from the group consisting of carbon black, charcoal, alumina, silica, barium silicate and barium sulphate.
- 9. A process according to claim 8, wherein the inert support is carbon black.
- 10. A process according to claim 6, wherein the amount of metal is between 0.1% and 5% relative to the weight of the inert support.
- 11. A process according to claim 6, wherein the amount of metal in the catalytic composition is between 1 and 1000 ppm relative to the weight of the silicone oil.
- 12. A process according to claim 1, wherein the first silicone oil is linear or cyclic and of average formula(e) (VII) or (VIII): wherein:the symbols R6 are identical or different and are a phenyl radical, linear alkyl radicals containing from 1 to 6 carbon atoms or branched alkyl radicals containing from 1 to 6 carbon atoms; the symbols X are identical or different and are R6, a hydrogen atom, a methoxy radical or an ethoxy radical; a, b and c are integers or fractions such that; 0<a≦1000 0≈b+c≦200 and at least one of the two groups X corresponds to a hydrogen radical if b+c=0, 1<a+b+c≦1000, d, e and f are integers or fractions such that: 0<d<10, and 1<e+f<10.
- 13. A process according to claim 12, wherein:0<a≦100 1<b+c≦100 1<a+b+c≦100; d, e and f are integers or fractions such that: 0<d<5, and 1<e+f<5.
- 14. A process according to claim 1, wherein the first silicone oil contains an epoxide.
- 15. A process according to claim 1, wherein at least one of the hydrosilylable functions in the stable silicone oil contains a “HALS” function. Marked-up amended claims according to 37 C.F.R. 1.121 are submitted in an attached document. Added matter is shown by underline and deleted matter is shown by strikethrough.
- 16. An anti-adhesive product for paper, glass or plastic comprising a silicone oil prepared by the process of claim 1.
Priority Claims (1)
Number |
Date |
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Kind |
96 15519 |
Dec 1996 |
FR |
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Parent Case Info
This application is a continuation application of application Ser. No. 09/319,843 filed on Aug. 16, 1999, now abandoned which is a 371 of PCT/FR97/02256 filed Dec. 10, 1997.
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58-152022 |
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Non-Patent Literature Citations (1)
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Continuations (1)
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Number |
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Parent |
09/319843 |
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US |
Child |
09/833928 |
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US |