High productivity alkoxylation processes

A technology of polyalkoxylation and polyoxyalkylene, applied in the field of polymerization, can solve the problems of increasing complexity and slow kinetic rate

Inactive Publication Date: 2008-08-06
BAYER MATERIALSCIENCE AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, such tubular reactors are not used for the production of polyethers because the slower kinetic rates of base catalysis require very large reactors, and because of th

Method used

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  • High productivity alkoxylation processes
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] In this example, calcium-based catalysts were prepared without aluminum alkoxides used in the preparation. A 250 ml three-necked flask reaction vessel was purged with nitrogen, and calcium hydroxide (9.75 g) was added together with TOMADOL 23-3 (106.2 g). The mixture was stirred at room temperature and 2-ethylhexanoic acid (2.23 g) was added by rapid dropwise addition over about 3 minutes. The reactants in the flask were heated to 30° C. in about 1 hour under stirring, and a vent was connected to the atmosphere through a reflux condenser. The contents of the flask were maintained at 30°C for an additional hour. Concentrated sulfuric acid (2.46 grams) was added to the flask at a rate of about 1 drop every 3 seconds. The contents of the flask were heated at 30°C for 15 minutes and an additional 2.46 grams of sulfuric acid was added at a rate of about 1 drop every 3 seconds. A reflux condenser was added to the three-necked flask and the contents of the flask were heated...

Embodiment 2

[0056] In this example, as described on page 31 of WO 04 / 18096 (Example B Reverse Phase Addition (LAPO)), in a 500 ml Lanthanum phosphate catalyst was prepared in a glass reactor. Lanthanum carbonate (15.6 g, 0.032 mol) was added to distilled water degassed with 100 mL of nitrogen (the solution was a slurry). A phosphoric acid solution was prepared by mixing 8.25 grams of 85% phosphoric acid (0.071 moles) into 100 milliliters of nitrogen degassed distilled water. Phosphoric acid was added to the carbonate solution at 25°C within 30 minutes. The solution was heated to 100°C for 2.5 hours. The product was cooled to room temperature and the solid was filtered.

[0057] The solid was transferred to a glass container and 250 mL of nitrogen-degassed distilled water was added at 50 °C for 30 min under rapid stirring. The product was cooled to about 25°C and filtered. The solid was transferred to a reactor and treated with ammonium hydroxide (5 mL, 10N) in water (250 mL). The co...

Embodiment 3

[0059] This example evaluates the modified calcium catalyst using a catch-up kinetic test. To the reactor was added nonylphenol 9.5 EO half batch (200 g), NEODOL 25 (200 g) and the catalyst mixture prepared in Example 1 DMC catalyzed C 12 3EO (14 g), heated to 100°C. The mixture was stripped at 100°C for 30 minutes, heated to 150-160°C and nitrogen blanketed to 30 psia. Ethylene oxide (286 g, 6.5 moles) was added over 2-4 hours. The total pressure (ethylene oxide and nitrogen) was maintained at less than about 60 psia. The mixture was digested at 150-160 °C until the baseline remained stable and the digestion process was continued for an additional 30 min. The mixture was cooled to 130°C, stripped for 20 minutes, and cooled to discharge temperature.

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Abstract

The present invention provides a continuous process for the preparation of a polyoxyalkylene polyether product of number average molecular weight N employing continuous addition of starter, involving a) establishing in a continuous reactor a first portion of a catalyst/initial starter mixture, b) continuously introducing into the continuous reactor one or more alkylene oxides, c) continuously introducing into the continuous reactor one or more continuously added starters, d) continuously introducing into the reactor fresh catalyst and/or further catalyst/further starter mixture, e) polyoxyalkylating combined starters by continuously practicing at least steps b) through d) herein until a polyoxyalkylene polyether product of number average molecular weight N is obtained and f) continuously removing the polyoxyalkylene polyether product from the continuous reactor. Modified-calcium hydroxide or modified calcium oxide and lanthanum phosphate catalysts exhibit catch-up kinetics and are thus useful for the production of polyalkylene oxides using the continuous and CAOS processes.

Description

[0001] This application claims priority to US Provisional Application No. 60 / 879212, filed January 8, 2007. technical field [0002] This invention relates generally to polymerization, and more particularly to an improved process for the production of polyoxyalkylene polyethers. Background technique [0003] In the past, a basic catalyst such as potassium hydroxide was used in the semi-batch process for the preparation of polyethers, the starter and the catalyst were added to the reactor, and a mixture of alkylene oxides or alkylene oxides was added in a certain way, thereby Simultaneously control heat release and polymer composition. These methods have been used for more than 50 years and have the advantage of producing products with narrow molecular weight distributions. The application technology of the polyol and ethoxylate industry is built around these narrow polydispersity products, making it difficult to introduce more economical methods unless these methods can pro...

Claims

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Application Information

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IPC IPC(8): C08G65/04C08G65/10B01F17/42C09K23/42C09K23/52
Inventor K·G·麦克答尼尔
Owner BAYER MATERIALSCIENCE AG
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