High stability concrete silicone joint glue and preparation method thereof
A high stability, concrete technology, applied in adhesives, polymer adhesive additives, non-polymer adhesive additives, etc., can solve the problems of easy pollution, increased crosslink density, increased modulus, etc., to achieve performance And the effect of improved stability, excellent plasticizing performance, and simple preparation method
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[0049] Preparation of raw materials:
[0050] Add 209.9g (4.58mol) of absolute ethanol and 500mL of petroleum ether into a 3L three-necked flask, keep the nitrogen flow rate at 0.1ml / min, stir evenly in an ice-water bath, control the internal temperature at about 10℃, and then add 300g dropwise (1.85mol) (chloromethyl)methyldichlorosilane, about 1h after the dripping is completed, continue to react at 40°C for 3h. Then, the solvent and unreacted ethanol were evaporated under a vacuum of 0.05Mpa, and then rectified under normal pressure to collect the product at 94-95°C to obtain 320g of colorless and transparent (chloromethyl)methyldiethoxysilane with a yield. 96%.
[0051] (Chloromethyl) methyl ethoxy butanone oxime silane preparation
[0052] Add 300g (1.85mol) (chloromethyl)methyldichlorosilane, 500ml petroleum ether and 387.2g (3.83mol) triethylamine into a 3L three-necked flask, stir well in an ice-water bath, and control the internal temperature at 10 ℃, then add 85.1g (1.85...
Embodiment 1
[0055] Put 290.8g (1.59mol) (chloromethyl)methyldiethoxysilane, 152.2g (1.75mol) morpholine, 178.2g (1.75mol) triethylamine, 0.4gKI and 800mL petroleum ether into a 3L three-necked flask After reacting at 60℃ for 4h under nitrogen protection. The generated triethylamine hydrochloride is filtered off, the filtrate is rotary evaporated to remove the solvent and unreacted triethylamine and morpholine, and then rectified to collect the product at 125-132°C / 10mmHg to obtain orange-yellow transparent (morpholinomethyl) ) 294.1 g of methyldiethoxysilane, with a yield of 79.4%.
[0056] 1 H NMR(300MHz, CDCl 3 ), δ3.67(4H), 3.60(4H), 2.45(4H), 2.20(2H), 1.10(6H), 0.16(3H)
[0057] Elemental analysis: C% 51.39, H% 9.88, N% 5.94.
Embodiment 2
[0059] Put 132g (0.5mol) (chloromethyl) methyl dibutyl ketoxime silane, 46.2g (0.53mol) morpholine, 53.6g (0.53mol) triethylamine, 0.2gKI and 300ml petroleum ether into a 1L three-necked flask After reacting at 75℃ for 6h under the protection of nitrogen, filter to remove the generated triethylamine hydrochloride, rotate the filtrate to remove the solvent and unreacted triethylamine, morpholine, and then rectify, collect 143-150℃ / 8mmHg The product obtained 118.2 g of orange-yellow transparent (morpholinomethyl) methyl dibutyl ketoxime silane with a yield of 74.9%.
[0060] 1 H NMR(300MHz, CDCl 3 ), δ3.63(4H), 2.40(14H), 2.18(2H), 1.08(6H), 0.18(3H)
[0061] Elemental analysis: C% 53.31, H% 9.25, N% 13.29.
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