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Manufacture of polytrimethylene ether glycol

A technology of methyl ether diol and diol applied in the field of polytrimethylene ether diol manufacture

Inactive Publication Date: 2008-08-20
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process also has the disadvantage that the polyether polyols obtained contain base catalyst residues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] This example describes the purification of polytrimethylene ether glycol using toluene as the added water immiscible solvent.

[0071] 1,3-Propanediol (11.9 kg) and 108 g of sulfuric acid were placed in a 22 L glass flask and then heated at 166 + / - 1 °C for 24 hours under nitrogen to produce polytrimethylene ether glycol. During the reaction, by-product water was removed by nitrogen sparging.

[0072] After the polymerization step, 4 kg of deionized water were added and the resulting mixture was kept at 95° C. for 4 hours under nitrogen to hydrolyze the ester formed during the acid-catalyzed polycondensation.

[0073] After hydrolysis, 2.6 kg of toluene was added, followed by stirring at 95°C for 10 minutes. Then stop stirring. It took about 20-30 minutes for the mixture to separate into two phases, with the organic phase at the top and the aqueous phase at the bottom.

[0074] Based on titration of the top layer sample, 4.0 grams of calcium hydroxide was added to th...

Embodiment 2

[0084] This example describes the preparation of polytrimethylene ether glycol using toluene as the added water immiscible solvent.

[0085] Polymerization of 1,3-propanediol was carried out as described in Comparative Example 2. After the polymerization step, 4 kg of deionized water were added and the resulting mixture was kept at 95° C. for 4 hours under nitrogen to hydrolyze the ester formed during the acid-catalyzed polycondensation.

[0086] After hydrolysis, 2.6 kg of toluene was added followed by stirring at 95°C for 10 minutes. Then stop stirring. It took about 20-30 minutes for the mixture to separate into two phases, the organic phase at the top and the aqueous phase at the bottom.

[0087] Based on the titration of the top layer sample, 5.0 grams of calcium hydroxide was added to the organic phase to neutralize the residual acid catalyst, followed by stirring at 70°C for 1 hour.

[0088] After neutralization, the mixture was filtered under nitrogen at 15 psig to ...

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PUM

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Abstract

A process of manufacture of polytrimethylene ether glycol comprising: (a) polycondensing reactant comprising diol selected from the group consisting of 1,3-propanediol, 1,3-propanediol dimer and 1,3-propanediol trimer or mixtures thereof in the presence of acid polycondensation catalyst to form polytrimethylene ether glycol; (b) adding water to the polytrimethylene ether glycol to form an aqueous mixture; (c) heating the aqueous mixture to hydrolyze acid esters formed during the acid catalyzed polycondensation; (d) adding to the hydrolyzed aqueous mixture organic solvent that is miscible with polytrimethylene ether glycol to form (i) organic phase containing the polytrimethylene ether glycol and residual acid polycondensation catalyst from the polycondensing and (ii) aqueous phase; (e) separating the aqueous phase and the organic phase; (f) adding base to the separated organic phase to neutralize the residual acid polycondensation catalyst by forming salts of the residual acid polycondensation catalyst; (g) separating the organic phase into (i) liquid phase comprising the polytrimethylene ether glycol, the organic solvent and any residual water, and (ii) solid phase comprising the salts of the residual acid polycondensation catalyst and the base which is unreacted; and (h) removing the organic solvent and the residual water from the liquid phase to obtain polytrimethylene ether glycol.

Description

field of invention [0001] The present invention relates to an improved method for purifying polytrimethylene ether glycol. technical background [0002] Polytrimethylene ether glycol and its use have been described in the art. A preferred method of preparing polytrimethylene ether glycol involves the acid-catalyzed polycondensation of 1,3-propanediol. For example, US6720459 discloses a continuous process for the preparation of polytrimethylene ether glycol from 1,3-propanediol using a polycondensation catalyst, preferably an acid catalyst. [0003] WO99 / 001496 discloses a process for the purification of polyethers comprising the steps of (a) heating polyether diols and water together for a period of time at a temperature sufficient to substantially hydrolyze the esters formed during polymerization, (b) separating the polyether from the water. ether, and (c) the polyether recovered from step (b) is further washed with hot water to remove residual acid. [0004] US200200070...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/34C08G65/46
CPCC08G18/4825C08G65/34C08G65/46
Inventor H·B·森卡拉吴宗灏郑威
Owner EI DU PONT DE NEMOURS & CO
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