Distillation: apparatus – Apparatus – Systems
Reexamination Certificate
2000-01-11
2002-06-04
Manoharan, Virginia (Department: 1764)
Distillation: apparatus
Apparatus
Systems
C202S169000, C202S203000, C203S041000, C203S043000, C203SDIG001, C210S295000, C210S664000, C564S437000
Reexamination Certificate
active
06398917
ABSTRACT:
DESCRIPTION OF THE BACKGROUND
DPPD is used on a large industrial scale as a stabilizer, inter alia, in the reaction of potassium methacrylate with 3-chloropropyltrimethoxysilane. In this application, the use of commercially available DPPD can impair product quality, in particular the color number of the product. Unfortunately, in the past, industrial quantities of DPPD have only been available on the market in a technical quality.
Crude DPPD, that is, commercially available DPPD or technically pure DPPD, has, as a rule, a purity in the range around 85% by weight, the remainder of about 15% by weight essentially consisting of unconverted or incompletely converted starting materials such as, for example, diphenylamine, and of inorganic components such as iron and chlorine, for example in the form of iron chloride. The commercial material is gray and is often in the form of a powder or in the form of flakes. In contrast thereto, pure DPPD is white and crystalline.
Several methods for the purification of DPPD are described in the literature. It is possible to crystallize DPPD from chlorinated hydrocarbons or carbon tetrachloride (Beilstein E III 13, 4
th
Auflage 1973, pages 115-118, The Merck Index, 9
th
Edition 1976, page 445). The disadvantage of these processes is, however, the use of chlorinated solvents which are toxic and pollute the environment.
Another purification method is solids distillation. This method can be applied successfully in the laboratory. For the purification of crude DPPD on an industrial scale, however, solids distillation is not a suitable process, since it is too expensive in engineering terms. A need therefore continues to exist for a method of inexpensively and effectively purifying DPPD.
SUMMARY OF THE INVENTION
Accordingly, one object of the present invention is to provide a process which allows crude DPPD to be purified in a simple and economical manner, thereby making a purified DPPD product available for application on an industrial scale.
Briefly, this object and other objects of the present invention as hereinafter will become more readily apparent can be attained in a process for purifying crude N,N′-diphenyl-p-phenylenediamine (DPPD), comprising extracting crude DPPD with a hydrocarbon or hydrocarbon mixture, passing the extract over an adsorption layer and recovering purified DPPD from this solution. Preferably, the purification is carried out under a blanketing gas.
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The Merck Index, Ninth Edition, 1976, p. 445.
Frings Albert-Johannes
Horn Michael
Jenker Peter
Monkiewicz Jaroslaw
Srebny Hans-Guenther
Degussa-Huels Aktiengesellschaft
Manoharan Virginia
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