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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: 2011-03-02
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] Put 1,3-propanediol (11.9 kg) and 108 g of sulfuric acid into a 22L glass flask, and then heat it under nitrogen at 166+ / -1°C for 24 hours to produce polytrimethylene ether glycol. During the reaction, by-product water was removed by nitrogen sparge.

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

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

[0074] Based on the titration of the top sample, 4.0 g of calcium hydroxide was added to the organic...

Embodiment 2

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

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

[0086] After the hydrolysis, 2.6 kg of toluene was added and then stirred at 95°C for 10 minutes. Then stop stirring. It takes 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.

[0087] Based on the titration of the top sample, 5.0 g of calcium hydroxide was added to the organic phase to neutralize the residual acid catalyst, and then stirred at 70°C for 1 hour.

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

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Abstract

The present invention relates to a process for manufacturing polytrimethylene ether glycol with improved purity.

Description

Invention field [0001] The invention relates to an improved method for purifying polytrimethylene ether glycol. technical background [0002] Polytrimethylene ether glycol and its applications have been described in the art. A preferred method of preparing polytrimethylene ether glycol includes acid-catalyzed polycondensation of 1,3-propanediol. For example, US6720459 discloses a continuous process for preparing polytrimethylene ether glycol from 1,3-propanediol using a polycondensation catalyst, preferably an acid catalyst. [0003] WO99 / 001496 discloses a method for purifying polyethers, including the following steps: (a) heating polyether glycol and water together at a temperature sufficient to substantially hydrolyze the ester formed during the polymerization process for a period of time, (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] US20020007043A1 describes a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/34C08G65/46
CPCC08G65/46C08G65/34C08G18/4825
Inventor H·B·森卡拉吴宗灏郑威
Owner EI DU PONT DE NEMOURS & CO
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