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Method for preparing polytetramethylene ether glycol by using imidazole polyoxometalate catalyst

A technology of polytetramethylene ether glycol and heteropolyacid imidazolium salt is applied in the field of preparing polytetramethylene ether glycol by using a heteropolyacid imidazolium salt catalyst, and can solve problems such as recovery efficiency and the like

Active Publication Date: 2013-10-23
杭州师恩科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] According to the present invention, in order to solve the problem of recovery efficiency of heteropolyacid catalyst in the reaction of tetrahydrofuran synthesis of PTMEG, especially phosphotungstic acid, phosphomolybdic acid, etc. have efficient catalytic effect for the reaction of tetrahydrofuran polymerization synthesis of PTMEG heteropolyacid, proposed A kind of method that prepares PTMEG by tetrahydrofuran by the catalyst of using ionic liquid heteropolyacid salt

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 15g of heteropolyacid imidazolium salt catalyst (phosphotungstic acid type) synthesized by the method described in the summary of the invention, add 30g of tetrahydrofuran with a water content of 0.15%, stir and dissolve to form a homogeneous reaction solution. Under the conditions of a temperature of 60°C and a stirring speed of 80-100 rpm, the reaction was carried out for 8 hours, and the yield and molecular weight of PTMEG in the reaction phase were detected by gel chromatography. After the reaction is completed, the reaction liquid is poured into a vacuum distillation equipment system for distillation recovery of tetrahydrofuran.

[0035] Sampling and detection of tetrahydrofuran content in the concentrate is 35% to 40% and the end point of concentration is reached. Add 1.2 times the volume of octane to the concentrate, stir for 1 hour, and settle to separate layers. The upper layer solution is octane-PTMEG-tetrahydrofuran. The tungsten content in the upper lay...

Embodiment 2

[0038] Take 15g of a commercially available phosphotungstic acid catalyst synthesized by a traditional method, add 30g of tetrahydrofuran with a water content of 0.15%, stir and dissolve to form a homogeneous reaction solution. Under the conditions of a temperature of 60°C and a stirring speed of 80-100 rpm, the reaction was carried out for 8 hours, and the yield and molecular weight of PTMEG in the reaction phase were detected by gel chromatography. After the reaction is completed, the reaction liquid is poured into a vacuum distillation equipment system for distillation recovery of tetrahydrofuran.

[0039] Sampling and detection of tetrahydrofuran content in the concentrate is 35% to 40% and the end point of concentration is reached. Add 1.2 times the volume of octane to the concentrate, stir for 1 hour, and settle to separate layers. The upper layer solution is octane-PTMEG-tetrahydrofuran. The tungsten content in the upper layer solution is detected to be 0.08%, and the l...

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Abstract

The invention relates to a method for preparing polytetramethylene ether glycol by using an imidazole polyoxometalate catalyst. The method belongs to the technical field of chemical synthesis. According to the invention, imidazole polyoxometalate is adopted as a catalyst, such that tetrahydrofuran is polymerized into polytetramethylene ether glycol (PTMEG) or a PTMEG copolymer or polytetrahydrofuran. The invention especially relates to PTMEG synthesis with the imidazole polyoxometalate catalyst modified with an ionic liquid method. Through improving the synthesis method, the synthesized imidazole polyoxometalate catalyst is different from a heteropolyacid catalyst synthesized with a traditional method. The difference mainly lies in the difference in phosphorus tungsten atom state forms. Traditionally, the heteropolyacid catalyst is in a molecular state. However, with the novel synthesis method, the imidazole polyoxometalate catalyst is in an ionic state, such that great difference is shown in specific application reactions. With the catalyst provided by the invention, reaction activity and catalyst recovery rates of the reaction are better than those of the heteropolyacid catalyst prepared with a traditional method.

Description

technical field [0001] The invention discloses a method for preparing polytetramethylene ether glycol using a heteropolyacid imidazolium salt catalyst, which involves a heteropolyacid catalyst to promote the polymerization of tetrahydrofuran into polytetramethylene ether glycol (PTMEG for short) or PTMEG copolymer or polytetramethylene ether glycol. The method of tetrahydrofuran, in particular, is to use the heteropolyacid imidazolium salt catalyst modified by the ionic liquid method to carry out the synthesis of PTMEG. It belongs to the technical field of chemical synthesis. Background technique [0002] PTMEG is one of the main raw materials for the production of spandex, high-grade thermoplastic polyurethane elastomers and other polyurethane products. [0003] In many prior disclosed technologies, heteropolyacids are used as catalysts to catalyze the ring-opening polymerization of tetrahydrofuran to produce PTMEG. [0004] Japanese patents No.S58-89081, No.S59-013523, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/20
Inventor 吕涛蔡天锡纪敏
Owner 杭州师恩科技有限公司
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