久久中文字幕美谷朱里,射吧亚洲

50-00-0 Synthesis

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142-04-1
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1208-52-2
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6582-52-1
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101-77-9 Synthesis

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Yield: 66.75 %Chromat. ， 0.085 %Chromat. ， 4.30 %Chromat.

Reaction Conditions:

Stage #1:formaldehyd;aniline hydrochloride in water at 38 - 90;
Stage #2: with sodium hydroxide in waterProduct distribution / selectivity;

Steps:

1
Example 1:; Hydrochloric acid (a concentration percentage by weight is 30.8%, this hydrochloric acid is a by-product from MDI apparatus) from storage tank 2 and aniline from storage tank 3 are fed into venturi mixer 5 by a pump 6 with a molar ratio of hydrochloric acid/anilin=0.36:1, for mixing and reacting with each other to produce aniline hydrochloride which is then pumped into circulation pipes and mixed with a circulation solution coming from a condensation stirred vessel 1 to obtain a mixed solution. The obtained mixed solution is introduced into a heat exchanger 7 to remove the reaction heat, and the mixed solution, which is cooled to 38°C and left the heat exchanger 7, is introduced into a feeding port of the high gravity rotating bed reactor 8 of rotating packed bed type. Formaldehyde solution (a concentration percentage by weight is 37 wt%) stream from storage tank 4 is fed through another feeding port of the high gravity rotating bed reactor 8, the ratio of formaldehyde to aniline is controlled at 0.40:1. The formaldehyde solution is mixed sufficiently with the previously mixed solution phase and conducted a pre-condensation reaction in the high gravity rotating bed reactor 8, the reaction temperature is controlled at 35°C, the reaction time is 0.5 sec, and the rotation speed of the rotor of high gravity rotating bed reactor is 1000rpm. Then the mixed reaction solution flows into the condensation reaction vessel 1 to proceed with the pre-condensation reaction, the temperature of reaction solution is controlled at 42°C, the stirring speed is about 110rpm, and the reaction residence time is about 20 min. Then the temperature of reaction solution is elevated to over 90°C to conduct a molecular rearrangement reaction, the residence time for molecular rearrangement reaction is about 2 hours. Finally a solution of diphenylmethylene diamine hydrochloride and polymethylene polyphenyl polyamines hydrochloride is obtained. 92 vol% of the reaction mixture from the condensation reaction vessel 1 returns to the circulation pipes, as circulation solution, and flows to heat exchanger 7, the other 8 vol% of the reaction mixture is discharged and neutralized with a sodium hydroxide solution at a concentration of 42 wt%. The salt water phase is separated from the polyamine organic phase, and the polyamines are washed with water and purified to finally obtain a mixture of diphenylmethylene diamine and polymethylene polyphenyl polyamines. The composition of products is listed in table 2.

References:

Ningbo Wanhua Polyurethanes Co., Ltd.;Beijing University Of Chemical Technology EP2145874, 2010, A1 Location in patent:Page/Page column 6

50-00-0 Synthesis

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62-53-3 Synthesis