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United States Patent (10) Patent No.: US 9,695.202 B2 Henning Et Al

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United States Patent (10) Patent No.: US 9,695.202 B2 Henning Et Al USOO969.5202B2 (12) United States Patent (10) Patent No.: US 9,695.202 B2 Henning et al. (45) Date of Patent: Jul. 4, 2017 (54) ORGANOMODIFIED SILOXANES HAVING 6,858,663 B2 2/2005 Knott et al. PRIMARY AMINO FUNCTIONS, NOVEL 29: R: 858. SE al ORGANOMODIFIED SILOXANES HAVING 7.3, 5 56 kNE al QUATERNARY AMMONIUM FUNCTIONS 7.96153 B2 3/2007 Burkhart et al. AND THE METHOD FOR THE 7,598,334 B2 10/2009 Ferenz et al. PRODUCTION THEREOF 7,612,158 B2 11/2009 Burkhart et al. 7,612,159 B2 11/2009 Burkhart et al. (71) Applicant: EVONIK DEGUSSA GMBH, Essen 7&7,619,035 B25 11/200950 HenningSE. et al. (DE) 7,754,778 B2 7/2010 Knott et al. 7,825,205 B2 11/2010 Knott et al. (72) Inventors: Frauke Henning, Eisen (DE): WilfriedWi- 7,825.2097,825,206 B2 11/2010 NeumannKnott et al. et al. Knott, Essen (DE); Horst Dudzik, 7.931,747 B2 4/2011 Weyershausen et al. Essen (DE) 8,138,294 B2 3/2012 Henning et al. 2002fO161158 A1 10, 2002 Burkhart et al. (73) Assignee:rsr rr Evonik Degussa GmbH, Essen (DE) 2008.OOO43572007/0128143 A1 6/20071/2008 GruningMeyer et et al. al. 2008/0125503 A1 5/2008 Henning et al. (*) Notice: Subject to any disclaimer, the term of this 2009.0137751 A1 5, 2009 Knott et al. patent is extended or adjusted under 35 38885 A. 29. R.enning et al.et al.al U.S.C. 154(b) by 82 days. 2010.0029587 A1 2/2010 Brickner et al. 2010.0041629 A1 2/2010 Giessler-Blank et al. (21) Appl. No.: 14/548,724 2010.0041910 A1 2/2010 Schubert et al. 2010, 0071849 A1 3/2010 Knott et al. 1-1. 2010.0081781 A1 4/2010 Schubert et al. (22) Filed: Nov. 20, 2014 2010/0105843 A1 4/2010 Knott et al. 2010/01 13633 A1 5/2010 Henning et al. (65) Prior Publication Data 2010/01.68367 A1 7, 2010 Schubert et al. 2010, O184913 A1 7, 2010 Ebbrecht et al. US 2015/0080593 A1 Mar. 19, 2015 2010/0249339 A1 9/2010 Henning et al. 2010/0292357 A1 11/2010 Knott et al. 2010/0298455 A1 11/2010 Henning et al. O O 2011/0021693 A1 1/2011 Henning et al. Related U.S. Application Data 2011/0034576 A1 2/2011 Henning et al. (62) Division- - - of application No. 13/521.351, filed as 20112011/0042004 0046305 A1 2/2011 Schubert et al. 2010, now abandoned. (Continued) (30) Foreign Application Priority Data FOREIGN PATENT DOCUMENTS Feb. 3, 2010 (DE) ........................ 10 2010 OO1531 EP 1956 038 8, 2008 GB 2 185984 8, 1987 JP 59-69110 A 4f1984 (51) Int. Cl. JP 62-185091. A 8, 1987 C07F 7/18 (2006.01) JP 63-5 1314. A 3, 1988 C08G 77/388 (2006.01) JP 5-295272 A 11, 1993 (52) U.S. Cl. JP 2008-31481 A 2, 2008 CPC .......... C07F 7/1804 (2013.01); CosG 77/388 " 2013-5 17337 A 5, 2013 (2013.01) OTHER PUBLICATIONS (58) Field of Classification Search CPC ... C08G 11/388; C08G 77/388: C07F 7/1804 International Search Report Issued Feb. 1, 2011 in PCT/EP10/70855 USPC .................................................. 556/418, 423 Filed Dec. 29, 2010. See application file for complete search history. (Continued) (56) References Cited Primary Examiner — Porfirio Nazario Gonzalez U.S. PATENT DOCUMENTS (74) Attorney, Agent, or Firm — Philip P. McCann; Smith Moore Leatherwood LLP 5,371,161 A 12/1994 Knott 5,384.340 A 1/1995 Hara et al. 5,430,166 A 7, 1995 Klein et al. (57) ABSTRACT 5.430,167 A 7, 1995 Klein et al. 5,455,367 A 10, 1995 Klein et al. 5,475,127 A 12/1995 Klein et al. The invention relates to a method for producing siloxanes 5,981,812 A 11/1999 Eufinger et al. selectively carrying primary amino groups by reacting them 6.255,511 B1 7/2001 Klein et al. with ammonia, and to compounds produced in this way. 6,291,622 B1 9, 2001 Dröse et al. 6,307,082 B1 10/2001 Klein et al. 6,489.498 B2 12/2002 Klein et al. 7 Claims, No Drawings US 9,695.202 B2 Page 2 (56) References Cited U.S. PATENT DOCUMENTS 2011 O230619 A1 9, 2011 Kuppert et al. 2011 O230633 A1 9, 2011 Ferenz et al. 2011/0245412 A1 10, 2011 Schubert et al. 2011/0281973 A1 11 2011 Schubert et al. 2011 03.01254 A1 12/2011 Knott et al. 2011/0306694 A1 12/2011 Glos et al. 2012fOO 10302 A1 1, 2012 Hartung et al. 2012fOO27704 A1 2, 2012 Henning et al. 2012, 0046486 A1 2, 2012 Henning et al. 2012fOO97883 A1 4, 2012 Henning et al. 2012/O190760 A1 T/2012 Henning et al. 2012/O190762 A1 T/2012 Hubel et al. 2012fO3O8494 A1 12, 2012 Schubert et al. OTHER PUBLICATIONS Japanese Office Action issued Mar. 10, 2014 in Patent Application No. 2012-551525 (English Translation only). Dow Corning, Silicones in Pharmaceutical Applications, 2001, Dow Corning Corporation, pp. 1-21, (24 pages in all, including Title page, blank page and concluding page.). US 9,695.202 B2 1. 2 ORGANOMODIFIED SILOXANES HAVING basically catalyzed equilibrium reactions of polysiloxanes PRIMARY AMINO FUNCTIONS, NOVEL with amino groups, silaZanes can also arise as by-products. ORGANOMODIFIED SILOXANES HAVING To increase the regioselectivity and avoid the formation of QUATERNARY AMMONIUM FUNCTIONS silaZane during the hydrosilylation of unsaturated amines AND THE METHOD FOR THE 5 with hydrogen siloxanes, use is made, according to DE PRODUCTION THEREOF 4436077 A1, of protective group technology, which requires two additional synthesis steps. Good selectivities during the This application is a divisional application of U.S. Ser. hydrosilylation of allylamine with tetramethyldisiloxane are No. 13/521,351 filed on Jul. 10, 2012, which is a 371 described in U.S. Pat. No. 5,026,890 A1 using the Karstedt 10 catalyst. Nevertheless, comparatively large amounts of at application of PCT/EP2010/070855 filed on Dec. 29, 2010. least 40 ppm of platinum are required by this platinum(0)- The invention relates to novel organomodified siloxanes divinyltetramethyldisiloxane complex. having primary amino functions and novel organomodified To produce methacrylamide-functional alkylsilanes, US siloxanes having quaternary ammonium functions and the 20050176911 A1 describes the reaction of epoxy-functional method for the production thereof. 15 alkylsilanes with methanolic ammonia solution at 0°C. to The production both of silanes and of organomodified 25° C. over 1 to 3 days. A subsequent derivatization with polysiloxanes having primary amino functions is described methacryloyl chloride leads to the target compounds. EP in the prior art by reference to the variety of synthesis routes. 1956038 A1 discloses a similar method for producing ter Aminoalkyl-functional alkoxysilanes are used as adhe minally methacrylamide-functional linear polydimethylsi sion promoters in coatings or adhesives and Sealants. They loxanes. Mixed-substituted polysiloxanes having additional are produced by the platinum(0)-catalyzed hydrosilylation functional groups are not mentioned. of allyl chloride, as is described, for example, in DE EP 1008614 A2 claims linear polydimethylsiloxanes, the 10.104966 A1. On account of secondary reactions, propene, chain ends of which are SiC-linked with in each case one chloropropane and propylchlorosilane are formed, meaning allyl polyether and one alkanolamine or alkanolalkylamine. that distillative purification of the product is required. The 25 The production takes place from a linear, epoxy- and haloalkyl function of the 3-chloropropylchlorosilanes polyether-functional polydimethylsiloxane by titanium obtained in this way can, according to EP 1273612 A1, be catalyzed epoxide ring opening for example with dietha further functionalized in diverse ways, for example by nolamine at 80° C. Polysiloxanes having primary amino reaction with ammonia, hydrogen Sulfide, alkali metal or functions cannot be produced by the described methods and ammonium sulfides, rhodanides and also methacrylates. By 30 are neither specified nor claimed. means of an alcoholysis, the functional chlorosilanes can be US 2008/0314518 A1 describes the reaction of amino converted to the corresponding alkoxysilanes. functional silanes or of ethylenediamine in situ with glyci For the more efficient production of aminoalkyl-func doxypropyltriethoxysilane for producing an aqueous two tional alkoxysilanes, in the prior art, instead of the three component adhesion promoter. The crosslinking required for stage chlorosilane route, the direct hydrosilylation of ally 35 good adhesion is ensured since an amino function reacts lamine with ethoxyhydrogen silanes is described. However, with more than one of the epoxide rings added in excess. this synthesis route has turned out to be difficult on account The prior art discloses siloxanes with not more than two of the strong inhibition of the transition metal catalyst by the amino functions and often without further functional groups. complexing allylamine. A series of patent applications dem Amino-functional siloxanes and in particular their charged onstrates the attempts to find an economical hydrosilylation 40 derivatives, which are accessible by reaction of the amino method with the help of specific ruthenium or rhodium function with various acids or else also by their alkylation to catalysts and also nitrogen and phosphorus compounds as give quaternary nitrogen compounds, have a marked elec cocatalysts, thus, for example, U.S. Pat. No. 4,481,364, U.S. trostatic affinity towards Surfaces and consequently provide Pat. No. 4,867,501, U.S. Pat. No. 4,921,988, U.S. Pat. No. for good substantivity of the compounds. The substantivity 4,927,953 or U.S. Pat. No. 5,001,246. The methods often 45 of the aminosiloxane, being its ability to anchor itself require large amounts of catalyst and lead, on account of electrostatically to Substrates, is associated with its func rearrangements of the double bonds and limited addition tionality density, i.e.
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