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Polytetramethylene ether glycol molecular weight distribution adjustment method

A technology of polytetramethylene ether glycol and number average molecular weight is applied in the field of adjusting the molecular weight distribution of polytetramethylene ether glycol, and can solve the problems of high cost, increased equipment size, difficulty in stirring power and the like

Active Publication Date: 2011-06-08
HYOSUNG CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the case of increasing the initial target molecular weight distribution to a certain value (e.g. 0.2) by adjusting the coordination number of the catalyst, it is difficult to predict the actual required stirring power
Therefore, this invention also has the disadvantage that it requires costly means that increase the size of the equipment

Method used

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  • Polytetramethylene ether glycol molecular weight distribution adjustment method
  • Polytetramethylene ether glycol molecular weight distribution adjustment method
  • Polytetramethylene ether glycol molecular weight distribution adjustment method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The THF monomer of 60kg is added in the reactor, and the phosphotungstic acid of 60kg and a small amount of water (its amount is the same as the molar number of the catalyst and the PTMG produced) are added therein. The reaction temperature of the reactor was maintained at 60°C, and THF monomer was fed constantly at a rate of 6 kg / hour. Meanwhile, by water feeder, in 12 hours, the moisture that total amount is 72ml is added in the reactor 6 times (that is, every 2 hours add the water of the amount of 12ml), stir reaction mixture in reactor simultaneously, The mixture is continuously transferred to a phase separator in order to separate the catalyst layer. Thereafter, water is recycled from the phase separator to the reactor so that the PTMG accumulates in the upper layer due to the formation of an overflow drain. After 24 hours of polymerization, the accumulated PTMG was sampled to measure the number average molecular weight and molecular weight distribution, and the r...

Embodiment 2

[0029] The THF monomer of 60kg is added in the reactor, and the phosphotungstic acid of 60kg and a small amount of water (its amount is the same as the molar number of the catalyst and the PTMG produced) are added therein. The reaction temperature of the reactor was maintained at 60°C, and THF monomer was fed constantly at a rate of 6 kg / hour. Meanwhile, by water supply, in 12 hours, the moisture that total amount is 72ml is added in the reactor 3 times (that is, every 4 hours add the water of the amount of 24ml), stir reaction mixture in reactor simultaneously, The mixture is continuously transferred to a phase separator to separate the catalyst layer. Thereafter, water is recycled from the phase separator to the reactor so that the PTMG accumulates in the upper layer due to the formation of an overflow discharge. After 24 hours of polymerization, the accumulated PTMG was sampled to measure the number average molecular weight and molecular weight distribution, and the result...

Embodiment 3

[0031]60 kg of THF monomer was added to the reactor, and 60 kg of phosphotungstic acid and a small amount of water (the amount was the same as, for example, the number of moles of the prepared PTMG) were added thereto. The reaction temperature of the reactor was maintained at 60°C, and THF monomer was fed constantly at a rate of 6 kg / hour. At the same time, through the water supply, a total amount of 72ml of water was added to the reactor in 2 pulses in 12 hours (that is, the water of 36ml was added every 6 hours). The reaction mixture was stirred such that the mixture was continuously transferred to a phase separator to separate the catalyst layer. Thereafter, water is recycled from the phase separator to the reactor so that the PTMG accumulates in the upper layer due to the formation of an overflow discharge. After 24 hours of polymerization, the accumulated PTMG was sampled to measure the number average molecular weight and molecular weight distribution, and the results we...

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Abstract

The invention relates to a method of preparing polytetramethylene ether glycol (PTMG) with molecular weight distribution (according to Mw / Mn ratio) 1.5 to 2.0; wherein, Mw represents weight average molar mass of PTMG, Mn represents number average molecular weight of PTMG; the invention in particular relates to a method of adjusting molecular weight distribution of the PTMG; wherein, the PTMG is prepared by adding water with predetermined amount in pulse mode as terminator in PTMG polymerization process. According to the invention, a method of preparing PTMG by tetrahydrofuran (THF) using heteropoly acid (HPA) catalyst layer comprises following steps of: preparing reaction mixture by adding THF, HPA catalyst and water into a continuous reactor; stirring the reaction admixture and adding THF and water with certain amount; wherein, the water is added in pulse mode; sampling the PTMG obtained in the reaction process to measure the number average molecular weight and molecular weight distribution.

Description

technical field [0001] The present invention relates to a process for preparing polytetramethylene ether glycol (hereinafter referred to as "PTMG") having a molecular weight distribution (in terms of Mw / Mn ratio) of 1.5 to 2.0, wherein Mw is the weight average molecular weight of PTMG, Mn is the number average molecular weight of PTMG, and the present invention particularly relates to a method for adjusting the molecular weight distribution of PTMG, wherein the PTMG is prepared by adding a predetermined amount of water in pulses as a terminator during the polymerization of PTMG. Background technique [0002] PTMG is a polymer used to make polyurethane, which is used as a raw material for spandex fibers, plastics or films. Depending on the use of polyurethane, various forms of polyurethane can be produced with a hard or soft segment structure, and depending on the use of polyurethane, it is required to have an optimal molecular weight or molecular weight distribution. Theref...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/20C08G18/48
CPCC08G65/10C08G65/20C08G65/2666C08G65/46
Inventor 吴俊锡李垠九白龙浩
Owner HYOSUNG CORP