A kind of diethyltoluenediamine synthesis method based on nano zinc oxide catalyst
A technology of diethyltoluenediamine and nano-zinc oxide is applied in the field of diethyltoluenediamine synthesis, and can solve the problems of easy deactivation of catalyst, low impurity content, catalyst service life, high reaction impurity content, etc.
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Embodiment 1
[0024] In the first step, add the catalyst to the autoclave and feed N 2 After replacing the air in the reactor, add toluenediamine and raise the temperature to 120°C; 2 Carry ethylene into the reactor, pressurize to 2.0MPa, react at 250°C for 1 hour, the molar ratio of toluene diamine to ethylene is 1:1.9; the weight of the catalyst is 0.2% of the weight of toluene diamine;
[0025] Step 2, after the reaction is over, press the reactant into the rectification tower for rectification treatment, the rectification adopts vacuum rectification, after the light components are distilled, diethyltoluenediamine is obtained at the bottom of the tower, and the vacuum rectification process The vacuum degree in the medium is 0.094MPa; the distillation temperature is 140°C, and the reflux ratio is 2:1;
[0026] The preparation method of described catalyst, comprises the steps:
[0027] S1, preparation of nano-zinc oxide carrier: dissolve urea and zinc chloride in aqueous ethanol, the con...
Embodiment 2
[0032] In the first step, add the catalyst to the autoclave and feed N 2 After replacing the air in the reactor, add toluenediamine and raise the temperature to 160°C; 2 Carry ethylene into the reactor, pressurize to 2.5MPa, react at 290°C for 4 hours, the molar ratio of toluenediamine to ethylene is 1: 2.3; the weight of the catalyst is 0.5% of the weight of toluenediamine;
[0033] Step 2, after the reaction is over, press the reactant into the rectification tower for rectification treatment, the rectification adopts vacuum rectification, after the light components are distilled, diethyltoluenediamine is obtained at the bottom of the tower, and the vacuum rectification process The vacuum degree in the medium is 0.098MPa; the distillation temperature is 170°C, and the reflux ratio is 4:1;
[0034] The preparation method of described catalyst, comprises the steps:
[0035] S1, preparation of nano-zinc oxide carrier: urea and zinc chloride are dissolved in ethanol aqueous sol...
Embodiment 3
[0040] In the first step, add the catalyst to the autoclave and feed N 2 After replacing the air in the reactor, add toluenediamine and raise the temperature to 130°C; 2 Carry ethylene into the reactor, pressurize to 2.2MPa, react at 280°C for 3 hours, the molar ratio of toluenediamine to ethylene is 1:2.2; the weight of the catalyst is 0.4% of the weight of toluenediamine;
[0041] Step 2, after the reaction is over, press the reactant into the rectification tower for rectification treatment, the rectification adopts vacuum rectification, after the light components are distilled, diethyltoluenediamine is obtained at the bottom of the tower, and the vacuum rectification process The vacuum degree in the medium is 0.094~0.098MPa; the distillation temperature is 150℃, and the reflux ratio is 3:1;
[0042] The preparation method of described catalyst, comprises the steps:
[0043] S1. Preparation of nano-zinc oxide carrier: Dissolve urea and zinc chloride in aqueous ethanol, the...
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