Amine titanium compound and preparation method thereof
A technology of titanium compound and dialkylamine, which is applied in the field of preparation of amine-titanium compound, can solve the problems affecting the transmission rate of the process, and achieve the effects of easy availability of raw materials, increased yield, and simple raw materials
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Embodiment 1
[0027] This embodiment is carried out in a 2L Schlenk bottle protected by an argon atmosphere, and all reagents used have been subjected to dehydration and deoxygenation treatment, and the steps are as follows:
[0028] Step 1: Add 800mL of n-hexane and 97g of N-ethylmethylamine to the Schlenk bottle in turn, and then add 2.5mol / L of n-butyl Lithium 610mL, stirred at room temperature for 5 to 10 hours to obtain n-hexane emulsion dissolved with lithium methylethylamide;
[0029] Step 2: Add 94g of titanium tetrachloride dropwise to the n-hexane emulsion prepared in step 1 at a rate of 1 to 3mL / min at -15 to -25°C, and raise the temperature to 40 to 60°C after the addition is complete. React for 12 to 24 hours to obtain tetrakis(methylethylaminotitanium);
[0030] Step 3: Add 7.5 g of hydrazine dropwise to the tetrakis(methylethylaminotitanium) obtained in step 2 at a rate of 1 to 3 mL / min at -15 to -25°C, and raise the temperature to 40 to 60°C after the addition is complete, ...
Embodiment 2
[0033] This embodiment is carried out in a 2L Schlenk bottle protected by an argon atmosphere, and the raw materials used are all treated with water and oxygen removal, and the steps are as follows:
[0034] Step 1: Add 700mL of n-hexane and 113g of diethylamine to the Schlenk bottle in sequence, then add 575mL of 2.5mol / L n-butyllithium dropwise at a rate of 1-3mL / min at -15~-25℃, and After stirring for 5 to 10 hours, the n-hexane emulsion dissolved with lithium diethylamide was obtained;
[0035] Step 2: Add 88g of titanium tetrachloride dropwise to the n-hexane emulsion prepared in step 1 at a rate of 1 to 3mL / min at -15 to -25°C, and raise the temperature to 40 to 60°C after the addition is complete. React for 12 to 24 hours to obtain tetrakis(diethylaminotitanium);
[0036] Step 3: Add 7.1 g of hydrazine dropwise to the tetrakis(diethylaminotitanium) obtained in step 2 at a rate of 1 to 3 mL / min at -15 to -25°C, and raise the temperature to 40 to 60°C after the addition ...
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