Process for preparing aminoalkylpolysiloxanes
A technology of aminoalkylpolysiloxane and aminoalkylsilane, which is applied in the field of preparation of aminoalkylpolysiloxane, and can solve the problems of unrecorded preparation, etc.
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Embodiment 1
[0109] The viscosity of 400 grams is 1000mm 2 / s (25°C), OH-terminated polydimethylsiloxane and 8.0 g of the hydrolyzate of the same OH-terminated aminopropylmethyldimethoxysilane (which has 8.5 meq / g of NH 2 concentration and an average chain length of 22 siloxy units) were mixed vigorously to form a highly turbid dispersion which was no longer transparent at layer thicknesses greater than 2 cm, so that the barcode could no longer be read.
[0110] While stirring using a paddle stirrer at about 300 rpm, the mixture was heated to 100° C. and the reaction of the two components was initiated by adding 40 mg of KOH as a 20% solution in ethanol. After 10 minutes the dispersion became clear and the catalyst was immediately deactivated with 42 mg of acetic acid. The reaction product (which was slightly cloudy due to potassium acetate) was cooled and then clarified by filtration. The obtained viscosity is 6700mm 2 / s (25°C), an amine oil with an amine density of 0.17 meq / g and a v...
Embodiment 2
[0122] The viscosity of 400 grams is 5900mm 2 / s (25° C.) of OH-terminated polydimethylsiloxane was mixed with 5 g of the aminoalkylsilane hydrolyzate in Example 1 to form a highly turbid dispersion and stirred as in Example 1, and It was heated to 90°C. After adding 100 mg KOH in 20% ethanol, the highly cloudy solution became clear after 21 minutes. Immediately thereafter, the catalyst was deactivated as described in Example 1; the slightly cloudy amine oil was clarified by filtration. At an amine content of 0.10 meq / g, the product has a volatility of 0.3% by weight and 19100mm 2 / s (25°C) viscosity.
[0123] A sample of this product was heat treated at 70°C for 7 days to test the tendency of the siloxanol groups to self-condense. Heat treatment causes viscosity increase to 30800mm 2 / s (25°C), meaning that the average chain elongation is only about 15%.
[0124] The thus obtained aminoalkylsiloxanes having a random distribution of dimethylsiloxane and aminopropylmethyl...
Embodiment 3
[0126] In order to check the practicability of the method under mild conditions, Example 2 was repeated at 60°C, but with double the amount of KOH. The reaction mixture took 54 minutes until the clear point was reached, and the catalyst was then deactivated (similarly to Example 2). Of course, at the same amine content, the volatility is still 0.3% by weight and the viscosity is 18700mm 2 / s (25°C). exist 29 In Si NMR, the fragment structure can no longer be detected at -22.40ppm, and its redistribution can be obtained smoothly even at a mild temperature of 60°C. It is evident from the low volatility that the equilibrium is reached long before this state .
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Abstract
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