DD246988A1 - DEVICE AND METHOD FOR CONTINUOUS PRODUCTION OF SODIUM N-BUTYLATE - Google Patents

Abstract

The invention relates to an apparatus and a process for the continuous production of sodium butylate solution in which aqueous technical sodium hydroxide solution and hydrous butanol are used. The reaction with simultaneous removal of water is carried out in a tray column, the design of which prevents the occurrence of deposits that impair the operation.

Description

The apparatus consists of a tray column (1) into which moist butanol preheated by partial condensation of the vapor in the dephlegmator (2) and aqueous caustic soda heated in a preheater (6) are fed via metering devices (7, 8) in the upper half of the column. The Dephlegmator a descending cooler (4) and a density separator (5) is connected downstream. The sump heater consists of a circulation evaporator (3).

The water from the caustic soda and the butanol and the water of reaction are constantly distilled off with the alcohol overhead. In this case, an approximately azeotropic composition is achieved. The turbulence occurring in certain soils, preferably in bell and sieve plates, flushes the passage opening constantly and prevents deposits. Thus, a constant efficiency of the soil is obtained and a continuous reaction is possible. These conditions are also ensured in the region of the column in which the caustic soda formed from the aqueous sodium hydroxide solution reacts with the butanol to Natriumbutylat. Since sodium hydroxide is relatively difficult to dissolve in butanol and, moreover, the impurities originating from the technical caustic soda tend, according to experience, to form compact deposits, this effect was not to be expected. ·

In the apparatus according to the invention can technical sodium hydroxide, the known impurities such. It is also possible to use butanol with a high degree of hydration, without the expectation of disturbances due to segregation and the like. The top product butanol / water is completely condensed in the heat exchanger (4) and separated in a densitometer (5). The resulting aqueous butanol is fed back to the colonnemitder necessary amount of fresh butanol. As a fresh butane oil, water-containing or dry butanol can be used. At the bottom of the device according to the invention is continuously withdrawn at a temperature of 132- ^: 140 ⁰ C 20-22% sodium butylate solution. The concentration is determined by the bottom temperature.

embodiments

Example 1: ·.

, In a semi-technical distillation apparatus (NW70), consisting of 6I glass flasks with electric internal heating, block tray column with 18 plates, dosing attachment, water separator and condenser, 0.3 kg / h of preheated butanol and 0.07 kg / h of 45% by means of metering pumps Sodium hydroxide solution on the 18th and 12th floor abandoned. From the bottom of the column 0.33 kg / h Natriumbutylatlösung be deducted. The bottom temperature is maintained at 137-138 ° C, the resulting butylate solution has a content of about 22% sodium butoxide.

Example 2:

A sieve tray column with 27 trays and 80 mm nominal diameter per hour 0.37 kg 45% preheated to 80 ⁰ C techn. Sodium hydroxide solution and 2.85 kg preheated to 90 ⁰ C butanol abandoned. The task of both components takes place on the upper floor. 1.8 kg of approximately 20% strength sodium butylate solution are removed at a temperature of 132-134 ° C. from the bottom of the column per hour. ''.

Example 3:

A G-cured bottom column with 40 trays and a nominal diameter of 1 000 mm will be heated 110 kg 45% per hour to 8O ⁰ C preheated techn. Sodium hydroxide solution and 1 190kg at 85 ° C. Preheated wet butanol (about 20% water) abandoned. The task of caustic soda takes place on the 22nd and the butanol on the 33rd floor. From the bottom of the column per hour 550 kg ca. 20% sodium butylate solution at a temperature of 136-138 C ³ are deducted. The sodium butylate solution contains less than 1% NaOH.

Claims (2)

Claim for the invention:. , 1. Apparatus and method for the continuous production of sodium n-butoxide from sodium hydroxide solution and n-butanol, characterized in that at 50 to 90 ° C, preferably at 80 to 90 ⁰ C, preheated aqueous sodium hydroxide solution in the upper half of a tray column , Preferably a sieve or G curls bottom column, and at 50 to 100 ⁰ C, preferably at 80 to 95 ° C, preheated n-butanol also in the upper half of the column, preferably in the upper third of the sodium hydroxide feed, in Ratio 1 to 4 to 12, preferably 1 to 7 to 11, fed and withdrawn continuously from the bottom of sodium n-butoxide at temperatures of 128 to 140 ⁰ C, preferably at 132 to 138 ° C. 2. Apparatus and method according to item 1, characterized in that aqueous technical sodium hydroxide solution with their known impurities and water-containing butanol to the saturation point, as well as the butanol distilled off from the tray column after the separation of the water, are used. For this 1 page drawing Field of application of the invention In the chemical industry, the production of alcoholates is required for a variety of reasons to carry out chemical processes. The preparation of sodium n-butoxide is a partial step in the production of butyl cyclopentanonecarboxylate from adipic acid butyl ester. , , The invention consists in a new device for the continuous recovery of sodium n-butoxide. Characteristic of the known technical solutions   It is known that it is possible to obtain alkali metal alcoholates if the corresponding alkali metal hydroxides are heated with an excess of the alcohol and the reaction water formed is distilled off continuously with the alcohol, an aid being e.g. Benzen can be added. The DRP 519443 describes this method. An improvement of this method is It. DRP 558469 in that a solution of alkali hydroxide in the alcohol in question is reacted in a column. DE 968903 describes a process in which the alkoxides are continuously prepared using a filled with packing distillation column of aqueous alkali hydroxide with the corresponding alcohol. In this case, the alkali metal hydroxide should deposit in solid form on the packing and then form the desired alkali metal alcoholate with the alcohol trickling down in the column. However, this method has the significant disadvantage that due to the depositions of solid sodium hydroxide and other impurities form compact deposits in a large area of the column, which lead to blockages after a short period of operation and stop the column. It is therefore not a technical solution for the production of 'sodium n-butoxide. DD-WP 202223 describes an apparatus for the continuous production of sodium n-butoxide from aqueous, technical sodium hydroxide solution and butanol using a rotary thin-film apparatus. In this method, both components are fed in DC. To secure the turnover very large surpluses of butanol 'are necessary here to remove the water of reaction. Object of the invention The aim of the invention is the continuous production of the condensate and other reactions versatile intermediate nat-n-butoxide under consideration of an economical use of energy and materials with safe process control. Explanation of the essence of the invention The invention has for its object to provide a device that allows continuous production of Natriumbutylatlösung, the disadvantages of other methods such as blockages of the column, high energy consumption, high material usage are largely avoided. Surprisingly, it has been found that the reaction in the device according to the invention, as shown in FIG. 1, can be realized using tray columns and while maintaining suitable process conditions for eliminating the disadvantages.