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Preparation method for phosphotungstic acid catalyst used for tetrahydrofuran polyreaction

A technology of tetrahydrofuran and phosphotungstic acid, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as quality reduction

Active Publication Date: 2011-11-02
HYOSUNG CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in such a production method, a part of the added hydrochloric acid remains in the phosphotungstic acid, which becomes an impurity during the THF polymerization reaction, and becomes a factor of quality reduction (such as discoloration of the polymer)

Method used

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  • Preparation method for phosphotungstic acid catalyst used for tetrahydrofuran polyreaction
  • Preparation method for phosphotungstic acid catalyst used for tetrahydrofuran polyreaction

Examples

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Effect test

Embodiment 1

[0030] After preparing the 1M mother liquor of sodium tungstate, as an additive, 1 L of strongly acidic cation exchange resin (HCR-H, Dow Chemical) was slowly added for 20 minutes to adjust the pH of the solution to 4. After the mother liquor whose pH value was adjusted to 4 was left at room temperature for 30 minutes, the mother liquor and the ion exchange resin were separated by filtration. The mother liquor is heated at a temperature of 80 to 90° C. for 1 hour, and then cooled. Phosphoric acid having an atomic ratio (P / W) of 12 was added, followed by stirring for 1 hour. Make the mother liquor pass through the ion exchange resin column (or tower) (diameter 40mm, length 1500mm) at a speed of 1.2L / hr. After filling 1.5 L of strongly acidic cation exchange resin (Amberject 1200H, Rohm & Haas) into the ion exchange resin column, sufficient pretreatment was performed with pure water. Collect the solution at the outlet of the ion exchange resin column until the measured pH is l...

Embodiment 2

[0032] The same treatment as in Example 1 was performed except that after preparing the 1M mother liquor of sodium tungstate, 2 L of zeolite (ZSM-5) was added as an additive, and the pH of the mother liquor was adjusted to 5.8.

Embodiment 3

[0034] The same treatment as in Example 1 was performed except that after preparing the 1M mother liquor of sodium tungstate, 100 g of phosphotungstic acid was added as an additive, and the pH of the mother liquor was adjusted to 4.5.

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Abstract

The present invention provides a method for preparing phosphor-tungstic acid catalyst which is used for preparing tetrahydrofuran polymer. Specifically, the invention provides the method which uses the alkaline tungstate that is taken as the principal raw material of catalyst for adjusting the reaction path. After the phosphor-tungstic acid catalyst with defectless Keggins structure is prepared, the catalyst is used for preparing THF single polymer or common polymer.

Description

technical field [0001] The present invention relates to the preparation method of the phosphotungstic acid catalyst that is used for tetrahydrofuran (THF) polymerization reaction, especially utilizes additive to adjust pH, so that use basic tungstate as raw material to form metatungstate (metatungstate) intermediate product, then prepare Method for phosphotungstic acid with Keggins structure. Background technique [0002] Commercially, phosphotungstic acid is mainly used as a catalyst in the homogeneous reaction of tetrahydrofuran to prepare polytetramethylene glycol. At this time, the higher the acidity of the phosphotungstic acid catalyst used, the higher its activity, especially when it has the Keggins structure, the acidity is the highest. Therefore, it is known that among phosphotungstic acid catalysts with various structures, phosphotungstic acid with Keggins structure is most suitable for preparing THF polymers. [0003] Generally, when preparing phosphotungstic aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/00C08G65/20
CPCB01J27/188B01J37/0009C08F4/22C08G65/10
Inventor 李垠九白龙浩许宰荣
Owner HYOSUNG CORP
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