Process for preparing a colourless solution of 3-(N-benzyl-2-aminoethyl)aminopropyltrimethoxy-silane hydrochloride in methanol
A process can prepare a colourless, methanolic solution of 3-(N-benzyl-2-aminoethyl)aminopropyltrimethoxysilane hydrochloride. The process includes, in step 1 fractionally distilling the vinylbenzyl chloride reactant component with addition of at least one stabilizer, and in step 2, metering and mixing the distillate (vinylbenzyl chloride) from step 1 into an initial charge of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and methanol in a molar ratio of the N-(2-aminoethyl)-3-aminopropyltrimethoxysilane to vinylbenzyl chloride of 1.0:0.80 to 1.0:1.15 and at a temperature in the range from 40 to 60° C. and leaving them to react further. The colourless, methanolic solution has an APHA colour number of <200 mg Pt—Co/l.
1. A process for preparing a colourless solution of 3-(N-benzyl-2-aminoethyl)aminopropyltrimethoxysilane hydrochloride in methanol, wherein the colourless solution has an APHA colour number of ≤200 mg Pt—Co/l, the process comprising:
fractionally distilling a vinylbenzyl chloride reactant component with addition of at least one stabilizer, to obtain a distillate containing vinylbenzyl chloride, and
metering and mixing the distillate from said fractionally distilling into an initial charge of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and methanol in a molar ratio of the N-(2-aminoethyl)-3-aminopropyltrimethoxysilane to vinylbenzyl chloride of 1.0:0.80 to 1.0:1.15 and at a temperature in the range from 40 to 60° C. and leaving them to react further.
2. The process according to claim 1 , wherein at least one stabilizer selected from the group consisting of nitromethane, 4-tert-butylpyrocatechol, and 2,4-dinitrophenol is used during said fractionally distilling.
3. The process according to claim 1 , wherein a vinylbenzyl chloride with APHA colour number≤5 mg Pt—Co/l is used during said metering and mixing.
4. The process according to claim 1 , wherein N-(2-aminoethyl)-3-aminopropyltrimethoxysilane is metered into vinylbenzyl chloride in said metering and mixing in a molar ratio of 1.0:0.99 to 1.0:1.01.
5. The process according to claim 1 , wherein N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and methanol are present in an initial charge in said metering and mixing in a molar ratio of 80:20 to 30:70.
6. The process according to claim 5 , wherein N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and methanol are present in the initial charge in a weight ratio of 70:30 to 40:60.
7. The process according to claim 5 , wherein N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and methanol are present in the initial charge in a weight ratio of 60:40 to 50:50.
8. The process according to claim 1 , wherein a product mixture present after the reaction in said metering and mixing is left to react further at a temperature in the range from 40 to 60° C. for a further period of 30 minutes to 3 hours while mixing.
9. The process according to claim 1 , wherein a composition obtained from said metering and mixing is diluted with addition of methanol.
10. The process according to claim 1 , wherein a composition obtained in said metering and mixing is adjusted to a content of 20% to 80% by weight of 3-(N-benzyl-2-aminoethyl)aminopropyltrimethoxysilane hydrochloride with addition of methanol.
11. The process according to claim 10 , wherein the composition obtained in said metering and mixing is adjusted to a content of 30% to 70% by weight of 3-(N-benzyl-2-aminoethyl)aminopropyltrimethoxysilane hydrochloride with addition of methanol.
12. The process according to claim 10 , wherein the composition obtained in said metering and mixing is adjusted to a content of 35% to 60% by weight of 3-(N-benzyl-2-aminoethyl)aminopropyltrimethoxysilane hydrochloride with addition of methanol.
13. The process according to claim 10 , wherein the composition obtained in said metering and mixing is adjusted to a content of 40% to 50% by weight of 3-(N-benzyl-2-aminoethyl)aminopropyltrimethoxysilane hydrochloride with addition of methanol.