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Caustic treatment of formaldehyde recycle column feed

A formaldehyde, distillation tower technology, used in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc.

Active Publication Date: 2014-08-06
INVISTA TEKSTAJLS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Not yet fully understood why the job appears to be running inefficiently

Method used

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  • Caustic treatment of formaldehyde recycle column feed
  • Caustic treatment of formaldehyde recycle column feed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] figure 2 is a graph showing the observed steam usage at the INVISTA LaPorte site with and without alkali addition in the feed to the recycle distillation column. The recycle distillation column (200) operates at a pressure range between 55-65 psig. The temperature at the feed point (160) is between 50-70°C, the bottoms (220) temperature is between 155-177°C, and the temperature at the top (240) is between 140-150°C. The reflux temperature was between 80-120°C and the reflux ratio was maintained at 0.5-0.8 (ratio of reflux to feed). figure 2 The graph in shows the steam consumption data for the recirculating distillation column. Tracks pounds of steam used per pound of crude BYD feed stream. Data were acquired during times when the pH of the BYD inlet stream was not adjusted and when the pH was raised by addition of aqueous sodium hydroxide (25-50 wt% NaOH). The average pH of the BYD inlet stream was observed to be about 5.35 prior to the addition of base. After a...

Embodiment 2

[0059] An improved method for removing formaldehyde from a crude butynediol product stream comprising the step of providing a crude butynediol stream containing butynediol and formaldehyde. The pH of the crude butynediol stream is then increased to form a treated product stream. The treated product stream is then passed to the inlet of the continuous distillation column. Finally, a concentrated formaldehyde stream is recovered from the distillation column overhead stream and a concentrated butynediol stream is recovered from the distillation column bottoms stream.

Embodiment 3

[0061] The procedure of Example 2 was repeated with additional steps. In this example, the pH of the treated product stream was raised to limit the reaction of butynediol and formaldehyde to form acetal complexes and to allow trace metals present in the treated product stream to become free of The level of reduced solubility in which the trace metals are precipitated in the treated product stream.

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Abstract

An improved method for removing formaldehyde from a crude butynediol product stream comprising the step of providing a crude butynediol stream containing butynediol and formaldehyde. A pH control agent is then mixed with the crude butynediol stream to form a treated product stream, wherein the pH of the treated product stream is raised to a level that limits the reaction of butynediol and formaldehyde to form acetal complex and decrease the solubility of trace metals. The treated product stream then flows into the inlet of a continuous distillation column. Finally, a concentrated formaldehyde stream from the overhead stream of the distillation column and a concentrated butynediol stream from the distillation bottoms stream that is essentially free of formaldehyde and acetal complex are both recovered.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS [0002] This application claims priority to US Provisional Application 61 / 563,875, filed November 28, 2011, the contents of which are incorporated herein by reference in their entirety. Field of Invention [0003] The present disclosure relates to a process for preparing 1,4 butynediol. More specifically, it relates to the improved efficiency during the distillation recovery of excess formaldehyde from crude 1,4 butynediol solutions. Background of the Invention [0004] 1,4-Butynediol (BYD) is a commonly prepared organic compound. BYD is a useful intermediate chemical in the preparation of pesticides, fabric additives, corrosion inhibitors, plasticizers, synthetic resins, butanediol, tetrahydrofuran, polyether polyols and polyurethanes. [0005] It is well known that BYD can be prepared by the Reppe method via the reaction of acetylene and formaldehyde. Some patents, such as US Pat. Nos. 2,300,969, 3,560,576, 4,093,668, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/80C07C29/88C07C33/046
CPCC07C29/80C07C29/88C07C33/046
Inventor 哈希姆·M·巴达特詹森·C·高斯
Owner INVISTA TEKSTAJLS