CS248574B1 - Bisphenolic aminosiloxanes - Google Patents

Abstract

Solution of siloxane resin description of general formula OH OH 5 / 20SI / CH2 / 5NHCH2CHCH2-N-CHCH 2 NH-CH 2 / CH 2 / 3sí03 / 2 wherein M represents a dian-based epoxy resin residue. The polymers are particularly suitable for the production of coatings on fibrous fillers for the release of plastics.

Description

X »248 574

The invention 8 relates to bisphenolic aminosiloxanes, suitable for surface modification of glass fibers and other fibers »

The quartz silicon polymers containing the most structurally phenolic nuclei known in the art are most commonly prepared by reacting diana-based epoxy resins with the appropriate organometallic derivative, e.g., tetraethoxysilane, organopolysiloxane / cp »88 334» 89 426 and 90 214 / »

The synthesis of aminoalkyltrialkoxysilanes and polyaminoalkyltri-alkoxysilanes (U.S. Pat. No. 3,560,543) discloses a further extension of silanes to modify the epoxy compositions. In these applications, aminosilanes are used as additives and hardeners for epoxy resins by kov 72 200 43kovkov »kovkov 171 Jap Jap Jap Jap aut Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap Jap 72 72 72 72 72 72 72 72 72 72 72 72 72 72 72 72 72 72 72 » or construction materials for the production of various products »Zq-crosslinking of these materials is most often achieved by crosslinking the use of polyamine & curing agents by reacting the active hydrogen amino group with the epoxy group»

Glass Fiber and Polyamide Resin Layered Insulation Eu constantly in Research Focus · These are to permanently withstand temperatures of 180 to 250 ° C and short-term to 400 ° C »For these reasons, it is necessary that the treatment not only improves fiber bonding but also to minimize thermal degradation »In application research, we have found that these problems can be effectively addressed by the use of siloxanes under the invention, which is advantageous to form in situ on the surfaces of the respective materials.

248 574

The invention describes bisphenolic aminosiloxanes of the general formula

OH OH 3 / 2OSi / OH2 / 3WH2OHOH2H2GH2GH (iH2NH / OH2Z3Si03Z2 where U represents the structure residue

S 0 to 2 »The preparation of these compounds can be accomplished by the # Adicius approach. The corresponding disilane is prepared by aminosilanes such as 3-aminoprepyl-triethoxysilane and dianium-based epoxy resin in the form of free epoxy groups. The hydrolyzous silane produces the corresponding unstable silantriol, which condenses to siloxane. is the easy availability of raw materials, with the greatest importance for the use of 3-aminopropyltriethoxysilane and liquid epoxy resins · The prepared thermosetting crosslinked siloxanes, in addition to the formation of in-thread fibers, can also be heterogeneous catalysts or substrates for the production of chromatographic carriers.

The invention is illustrated by the following Examples

81.4 g of 3-aminopropyltriethoxysilane and 64 # 9 g of isopropyl alcohol were introduced into the flask. At 50 ° C, 70 g of dianium-based epoxy resin containing 3.488 S74 epoxy groups of 0.515 mol / LOOg and a viscosity at 25 were added slowly with stirring. ° C 13 725 mP · * e and stirred for 1.5 h · The prepared 70% adduct solution has a viscosity at 20 ° C 260 mPa · s 5 g of water were added to 50 g of adduct solution 8a and the composition was poured into the mold. h free pre-drying hardened at 145 ° 0 6 h «Prepared siloxane is a clear hardness of 12 according to ČSN 673075« η ^ θ «1.5091 * Measurement of thermal stability was performed on a Derivatograph MOtó / MÍ / the temperature of 5eG / min * the weight of the individual temperatures is given in Table 1 «

Table 1 Working temperatures * Z ° OZ \ _ 250 300 400 500 600 700 1000 t Weight loss Z% Z 2.0 3.5 13.2 23.4 '32.4 40.0 40.0

The aminosiloxane coating was formed on carbon fibers by application of a 5% solution of adduct in water at pH 3.6 followed by drying for 4 hours at 125 ° C. &Quot; 30% " masses · The results obtained are shown in Table 2 for comparison with non-treated carbon fiber N «

Table 2

siloxane N tensile strength elongation Z% / -xmax- 11.4 - 19 * 0 flexural strength Z MPa Z - 94.6 66.9 flexural modulus Z MPa Z 5 497 1 612 notch toughness z kj / k2 / ______ 6,6_aa 4 248 574 ball hardness ZN / mm2 / 106.7 89.7

The glass fabric was treated with 1% aminosilane solution and cured at 12 ° C for 6 hours to form 3-aminopropylsiloxane in situ. The same procedure was followed by coating the bisphenolic aminosiloxane. with 3-aminopropylsiloxane the flexural strength is 3 000 h at 220 ° CS 230 MPa, after 2000 h at 24 ° 0 390 MPa · In the case of bisphenolic aminosiloxane the flexural strength is 3000 h 22 ° C 550 MPa, after 2000 h at 240 ° C 560 MPa »Example 2 4 g of water was added to 50 g of 70% epoxy resin disilane with an average molecular weight of 480 and 3-aminopropyltriethoxysilane in an isopropylalcohol. Example 1 prepared siloxane with a hardness of 12 µm 10 1.5105 * The thermal stability results are shown in Table 2 ·

Table 2 Working Temperature / ° Q / 200 260 300 400 Weight Loss /% / 0.8 2.0 3.5 10.5 Example 3 To 50 g of 50% epoxy resin disilane with an average molecular weight of 650 and Of 3-aminopropyltriethoxysilane in isopropanol was added 1.5 g of water. By the procedure of Example 1, a siloxane having a hardness of 11 and 1.5133 was prepared. The results of the thermal stability are shown in Table 3.

Table 3 Temperature of Temperature / ° S / Weight Loss i% / 260 300 _ 400 2 * 6 8.1 1.2

Claims (1)

I FOR DME T V.X N I I E E 248 574 Biaphenolic aminosiloxanes of general OH OH 1 1, / 20Si / aH2 / 3NH3H20tt212 - «- 0H2QHaH2RH / 0H2Z3Si03 / 2 where they represent the structure residue Printed Moravian Printing Works, Center. 11 100, tř.Lidových milicí 3, Olomouc Price: 2,40 Kčs