Preparation method of aliphatic diamine with high steric hindrance effect
An aliphatic binary, high steric hindrance technology, which is applied in the fields of special chemicals and fine chemicals, can solve the problems of low purity and high functionality of curing agents, and achieve good yellowing resistance
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[0025] The method of preparing an aliphatic dicarboxylic secondary amine a high hindrance: Example 1
[0026] Object of the present invention is to provide a high product yield, high purity, ease of operation, linear low reactivity of toxic pollution / branched chain aliphatic dibasic secondary amine environmentally friendly production method. Desired product while significantly lower reactivity, good flexibility can be imparted to the article.
[0027]This secondary amine on the α-position carbon has an amino group substituted with two alkyl groups, i.e. substituent groups belonging to a secondary carbon atom on the N-substituted alkyl group, obvious steric effects, effectively reduce the reactivity of the secondary amino group. And gives good flexibility products. However, synthetic aliphatic dibasic secondary amine containing large alkyl substituent on an amino group with a certain degree of difficulty.
[0028] Structural formula of the present invention synthesized aliphatic ...
Example Embodiment
[0048] Example 2: preparation of secondary amines aliphatic dicarboxylic high a hindrance
[0049] The 1,4-diamine 88.2 g (1.0 mol), diisobutyl ketone 426.7g (3.0 mol) and 0.9 g platinum on carbon catalyst were added to a stainless steel high pressure reactor vessel, the closing doghouse, the reaction vessel was replaced with nitrogen the air was replaced with hydrogen three times and three times with nitrogen, heating up, temperature was controlled at 60 ℃, a hydrogen pressure of not higher than 6.0 MPa, under the reaction conditions for 10 hours gradually raising the temperature, the maximum reaction temperature is controlled at 92 deg.] C or less , total 25H reaction, cooling to 28 ℃, venting exclude hydrogen replaced with nitrogen and the residual hydrogen gas, returned to normal pressure. The reaction product was filtered, the catalyst residue, recycling. The filtrate was washed with water ring vacuum distillation under reduced pressure, at a low temperature to an excess keto...
Example Embodiment
[0051] The method of preparing an aliphatic dicarboxylic secondary amine a high hindrance: Example 3
[0052] The 1,5-diamine 102.8g (1.0 mol), 2,4- dimethyl-3-pentanone 274.1g (2.4 mol) and palladium on charcoal catalyst 5g into a high pressure stainless steel reactor, with nitrogen substitution reaction air in the container 3. After nitrogen was replaced with hydrogen 3 times, heating, controlling the hydrogen pressure 3.0 ~ 3.5 MPa, the initial reaction temperature was 60 ℃, as the reaction proceeds the temperature may be gradually increased, the maximum reaction temperature within 95 deg.] C, a hydrogenation reaction was 20 hours , cooling, hydrogen gas vented, and the residual hydrogen was replaced with nitrogen, returned to normal pressure. The reaction product was filtered, the catalyst residue, recycling. First distilled off excess 2,4-dimethyl-3-pentanone, and the water by-product 2,4-dimethyl-3-pentanol under reduced pressure, and then increasing the temperature to remov...
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