Cleaning and liquid contact with solids – Processes – Hollow work – internal surface treatment
Reexamination Certificate
2000-04-18
2003-05-27
Gulakowski, Randy (Department: 1746)
Cleaning and liquid contact with solids
Processes
Hollow work, internal surface treatment
C134S002000, C134S022110, C134S022100, C134S016000, C134S017000, C134S025100
Reexamination Certificate
active
06568406
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method for cleaning plant parts which are used for the preparation or processing of (meth)acrylic esters.
2. Description of the Background
(Meth)acrylic esters are produced on a large industrial scale generally by esterifying (meth)acrylic acid with alkanols in the presence of strong acids and, if required, an entraining agent for removing the water of the esterification. The synthesis is preferably carried out in stirred reactors with attached distillation columns, and the working-up with the aid of a plurality of distillation columns and extraction apparatuses (cf. Kirk Othmer, Encyclopedia of Chemical Technology, 4th Ed., Vol. 1, pages 301-302). Heat is supplied and cooling effected usually by means of heat exchangers, such as plate-type, tube-bundle or spiral heat exchangers or circulation evaporators. The distillation columns are provided with baffles, such as sleve trays, bubble caps, dualflow trays or stacked packings or contain packing.
One problem in the preparation of (meth)acrylic esters is the considerable tendency of the (meth)acrylic compounds to undergo free radical polymerization, especially under the action of heat or light. Especially in the esterification, reaction temperatures from 80 to 140° C. are generally necessary in order to achieve economical esterification rates. In the purification, the necessary separation of the low-boilers and high-boilers by distillation and the isolation of the target ester require temperatures of from 60 to 150° C. Thus, the esters are exposed to terminal loads which can easily trigger an undesired polymerization. Soiling of the preparation apparatus and of the distillation columns and blockage of the lines, pumps, evaporators (fouling) and condensers by polymers are generally the result.
Particularly with the use of crude acrylic acid, which is preferred for economic reasons and also contains various carbonyl compounds, such as formaldehyde, acetaldehyde, furfurals, benzaldehyde, protoanemonin and dicarboxylic acids, such as maleic acid or itaconic acid, soiling and blockage of plant parts occur to an increasing extent.
In order to prevent the undesired free radical polymerization, inhibitors are added to the reaction mixture.
However, complete elimination of polymer formation therewith is not achievable. After an operating term of several weeks, it is therefore usually necessary to free plant parts from polymer.
Another complicating factor is that relatively high molecular weight compounds, as formed by repeated Michael addition reactions of the (meth)acrylic acid with the (meth)acrylate, increase the viscosity of the reaction mixture and facilitate the position of polymer in plant parts.
The cleaning of the plants, for example by treatment with solvents or by manual removal of the polymer, is a complicated, expensive process causing environmental pollution. The plant parts are usually cleaned by treatment with suitable organic solvents, for example dimethylformamide, dibutylformamide, dimethylacetamide, dibutylacetamide, sulfolane or N-methylpyrrolidone. The solutions obtained have to be disposed of by a complicated procedure. In addition, manual removal of the polymer, for example from distillation trays or from evaporator pipes, may be necessary.
In addition to the environmental pollution as a result of the cleaning, the polymer formation and the cleaning of the plant parts always also result in a loss of desired products, since residual amounts of starting materials and desired esters remain in the plant after emptying. Moreover, the availability of the production plant is reduced as a result of the necessary shutdown.
For economic and ecological reasons, cleaning of the plant by a different method and substantial avoidance of losses of desired products should therefore be strived for.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a method for cleaning plant parts which are used for the preparation or processing of (meth)acrylic esters, which method avoids the above disadvantages.
We have found that this object is achieved in a novel method by
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
(a) emptying the plant parts,
(b) flushing the plant parts with aqueous 5 to 50% strength by weight alkali metal hydroxide solution,
(c) removing the alkali metal hydroxide solution from the plant parts,
(d) if required, washing the plant parts with water and
(e) if required, drying the plant parts.
Before the washing with alkali metal hydroxide solution, the plant parts are emptied as completely as possible so that only very small amounts of reaction mixture or of substance present in the plant part remain behind.
The concentration of the alkali metal hydroxide solution used is preferably from 10 to 30% by weight, based on the weight of the prepared solution.
Preferably, the temperature of the alkali metal hydroxide solution during flushing is from 20 to 140° C., particularly preferably from 60 to 100° C. It should be ensured that the alkali metal hydroxide solution is at this temperature during contact with the polymers deposited in the plant parts. If the entire plant is heated to the corresponding temperature, the temperature of the alkali metal hydroxide solution used corresponds to this desired temperature. If plant parts are not heated to this temperature, the temperature of the alkali metal hydroxide solution used should be adjusted so that the stated temperature prevails in the areas with the polymer coating.
If necessary, the temperature of the alkali metal hydroxide solution is chosen correspondingly higher during introduction into the plant.
Sodium hydroxide is preferably used as the alkali metal hydroxide. The alkali metal hydroxide solution can be circulated through the corresponding plant parts in order to achieve a sufficiently long treatment time. The treatment time is usually from 1 to 24 hours, depending on the level of deposits in the plant parts. The treatment time, the concentration of the alkali metal hydroxide solution and the temperature depend on the type of (meth)acrylic ester used in the plant part and on the type and amount of the polymer. Usually, (meth)acrylic esters of alcohols, such as alkanols of 1 to 12, preferably 1 to 8 carbon atoms, are prepared by direct esterification or transesterification. Examples of alkanols are methanol, ethanol, n-butanol, 2-ethylhexanol and dimethylaminoethanol.
The (meth)acrylic esters can also be obtained by reacting olefins, preferably isobutene, with (meth)acrylic acid.
The plant parts to be cleaned are those plant parts which come into contact with the starting materials or products during the preparation or processing of (meth)acrylic esters, in particular during the esterification of (meth)acrylic acid with alkanols. The plant parts may be, for example, reactors, distillation columns, extraction apparatuses, heat exchangers, evaporators, condensers, pipes or pumps, which may be connected to form a unit. Preferably, the connected plant parts comprise a distillation unit which has a flushing line between the evaporator and the top of the columns. In particular, polymers formed in the preparation and processing of (meth)acrylic esters are deposited in these plant parts. The treatment with the alkali metal hydroxide solution causes or at least partly, hydrolysis of the ester groups of the (meth)acrylate polymers, resulting in liberation of the alkanol component. Inter alia, the polymer is detached from the plant parts as a result of this and goes completely or partly into solution and can thus be discharged with the alkali metal hydroxide solution from the plant parts.
To ensure that distillation apparatuses can be readily cleaned with the alkali metal hydroxide solution, they are preferably equipped with their own flushing lines. These permit the transport of the alkali metal hydroxide solution, which is heated, for example, in the evaporator of the column, to the top of the column. The flushing lines enable the top of the column and all column t
Aichinger Heinrich
Herbst Holger
Nestler Gerhard
Schröder Jürgen
BASF - Aktiengesellschaft
Gulakowski Randy
Winter Gentle E.
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