Room-temperature vulcanisable organopolysiloxane compound to give an elastomer and novel organopolysiloxane polycondensation catalysts
一种缩聚催化剂、聚硅氧烷的技术，应用在有机化学等方向，能够解决催化剂不能用、少工业开发、有毒等问题
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Embodiment 1
[0156] Example 1: Synthesis of catalysts (5) and (6) according to the invention
[0157] a) synthesis of catalyst (5):
[0158] [Zn (isopropyl acetoacetate) 2 ] or [Zn(iPr-AA) 2 ], where iPr-AA = isopropyl acetoacetate anion or enolate anion of isopropyl acetoacetate
[0159] A 97% solution of 100 mmol sodium methoxide (6.12 g) in 100 ml isopropanol was concentrated 20% by distillation, then 95% 100 mmol isopropyl acetoacetate (15.93 g) was added and the solution was heated at 80 °C for 1 Hours, an orange homogeneous solution was obtained. A solution of zinc chloride (50 mmol, 7 g) in 50 ml isopropanol was then added at 70° C. within 1 hour. Heating is maintained between 80 and 90° C. for 3 hours and 30 minutes, and then, after cooling, the sodium chloride formed is filtered. The alcoholic solution was evaporated to dryness to obtain 25.3 g of a paste which was dissolved in 200 ml of ethanol. After hot filtration and evaporation to dryness, 17.2 g of white solid were...
Embodiment 2
[0167] Example 2: Initial Test
[0168] - Catalyst (3): Zn(DPM) 2 or [Zn(t-Bu-acac) 2 ], where (t-Bu-acac)=2,2,6,6-tetramethyl-3,5-heptanedione anion or 2,2,6,6-tetramethyl-3,5- Enolate anion of heptanedione,
[0169] - Catalyst (4): [Zn(EAA) 2 ], where EAA=ethyl acetoacetate anion or enolate anion of ethyl acetoacetate,
[0170] - Catalyst (5): [Zn(iPr-AA) 2 ], wherein iPr-AA = isopropyl acetoacetate anion or enolate anion of isopropyl acetoacetate, and
[0171] - catalyst bis(2,2,7-trimethyl-3,5-octanedione)zinc of formula (6):
[0172]
[0173] To demonstrate the catalytic activity of the new substance, two simple tests were developed.
[0174] In both tests, proceed in the following way:
[0175]- the functionalized or unfunctionalized oil, then the catalyst, then the crosslinker in the case of RTV2, and then optionally water are added successively to a small open cylindrical vessel equipped with a magnetic stirring bar, And set the stirring at 300rpm. Measu...
Embodiment 3
[0198] Example 3: Paste tests for RTV1 and RTV2
[0199] Certain catalysts were then also tested in more compact (plus proches) systems called "pastes".
[0200] In RTV1, the paste used was prepared as follows: a mixture of 3464 g of α,ω-dihydroxylated oil and 120 g of vinyltrimethoxysilane with a viscosity of 20,000 centipoise containing 0.066% OH was prepared under stirring. 16g of a 2wt% solution of lithium hydroxide in methanol was added, followed after 5 minutes by 400g of AE55 fumed silica. The mixture was freed of volatile components under vacuum and then stored in a moisture-free environment.
[0201] For each test, the catalyst tested was mixed with 50 g of this paste, and the catalytic ability was then evaluated in three ways (see results in the table below):
[0202] - tack-free time (SOT) at the end of which surface crosslinking is observed on a 2 mm film;
[0203] - Persistence of tackiness to the touch at 48 hours;
[0204] - Hardness of 6 mm thick wire (Sh...
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