Methylene-crosslinked polyarylamine and process for preparing same

• US 5,053,539 A
• Filed: 01/17/1991
• Issued: 10/01/1991
• Est. Priority Date: 04/11/1990
• Status: Expired due to Term

• Current Assignee: Mitsui Chemicals Incorporated (Mitsui Chemicals)
• Original Assignee: Mitsui Toatsu Chemicals Incorporated (Mitsui Chemicals)
• Inventors: Nagayoshi, Tatsuya, Nagou, Takashi, Ishida, Noritoshi, Nagamatsu, Katsuyuki, Yano, Naoyuki, Itoh, Hiroyuki, Tashima, Zunzi
• Primary Examiner(s): Siegel, Alan
• Assistant Examiner(s): NOT, DEFINED
• Application Number:
  US07/642,338
• Time in Patent Office: 257 Days
• Field of Search: 564/333, 564/331
• US Class Current: 564/333
• CPC Class Codes: C07C 209/78 from carbonyl compounds, e.g. from formaldehyde, and amines having amino groups bound to carbon atoms of six-membered aromatic rings, with formation of methylene-diarylamines

Abstract

A methylene-crosslinked polyarylamine is disclosed which contains a less amount of N-methylmethylenedianiline. A process for continuously preparing this kind of methylene-crosslinked polyarylamine is also revealed which comprises reacting aniline with formalin in the presence of hydrochloric acid under specific reaction conditions.

Claims

1. A process for preparing a methylene-crosslinked polyarylamine by reacting aniline with formalin in the presence of hydrochloric acid under the following conditions (a), (b), (c) and (d):

(a) the amount of hydrochloric acid is in the range of from 0.1 to 0.5 mole per mole of aniline;

(b) the amount of aniline is in the range of from 1.5 to 4.0 moles per mole of formalin;

(c) the reaction is divided in at least four stages, and

the reaction in the first stage is carried out at 20 to 50°

C. in a water/aniline ratio in the range of from 1.3 to 2.5 moles,

the reaction in the second stage is done at 40 to 70°

C. in a water/aniline ratio in the range of from 1.9 to 5.0 moles,

the reaction in the third stage is done at 50 to 90°

C. in a water/aniline ratio in the range of from 2.4 to 5.7 moles, and

the reaction in the last stage is done at a temperature of 110°

C. or more; and

(d) formalin is divided into 3 or more stages and used in the reactions in the respective stages.

2. The process for preparing a methylene-crosslinked polyarylamine according to claim 1 wherein prior to being fed to the first stage, formalin is mixed with hydrochloric acid, and in the second et seq. stages, formalin is fed to each reaction system in the concentration range of from 10 to 25%.