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Method for preparing polyether polybasic alcohol with narrow molecular weight distribution

A narrow molecular weight distribution, polyether polyol technology, applied in the field of polyether polyol preparation

Active Publication Date: 2004-07-07
HODOGOYA CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

All in all, there are industrial drawbacks in the above-mentioned methods

Method used

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  • Method for preparing polyether polybasic alcohol with narrow molecular weight distribution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 to 3

[0040] With the sample of 100 parts, the polytetrahydrofuran [hydroxyl value=119.4mg KOH / g that makes with fluorosulfonic acid catalyst in known method; Number average molecular weight=940; Bulk viscosity=2.82 poise (40 ℃); Molecular weight distribution ( Mvis / Mn)=2.06], 100 parts of tetrahydrofuran and 100 parts of 30% sulfuric acid aqueous solution join in the 500-cc four-necked flask (there is thermometer and stirrer housed, and each mouth all uses independent cock closure), and in The mixture was stirred and mixed at 70° C. for 30 minutes, and then separated into two phases by standing. The next phase is an aqueous sulfuric acid phase, which is removed by liquid-liquid separation. The upper organic phase was neutralized with calcium hydroxide and the tetrahydrofuran was evaporated off. 100 parts of toluene were added to this organic phase and allowed to azeotropically dehydrate. Filtration was performed with a filter aid, and toluene was evaporated from the filtrate unde...

Embodiment 4

[0043] 125 parts of samples were treated with acetic anhydride-perchloric acid (HClO 4 ) catalyst prepared polytetrahydrofuran [hydroxyl value = 66.0mg KOH / g; number average molecular weight = 1700; bulk viscosity = 10.57 poise (40 ℃); A 30% sulfuric acid aqueous solution was stirred and mixed at 70° C. for 30 minutes, and then an extraction operation was performed. Treatment was performed in the same manner as in Example 1. The results for the products obtained here are given in Table 2 below.

[0044] Example

Embodiment 5 to 7 and comparative example 1

[0046] Put 400 parts of tetrahydrofuran in a 1-liter four-necked flask (equipped with a thermometer and a stirrer), and then add 4.0 parts of antimony pentachloride (SbCl 5 ). Then 80 parts of 30% oleum were added within 2 hours and the monomer was further polymerized at 0° C. for 4 hours. The polymerization solution was divided into 4 parts, and 122 parts of [Comparative Example], 46 parts, 41 parts or 27 parts of water were added to each part to control the concentration of sulfuric acid therein. The fractions were mixed and stirred with water at 60°C for 60 minutes and then left to stand still for fractional extraction.

[0047] Next, it was treated in the same manner as in Example 1, and the properties of the polytetrahydrofuran thus prepared as Comparative Example 1 and Examples 5, 6 and 7 are shown in Table 3 below.

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Abstract

The method for preparing polyether-polyol having a narrow molecular distribution comprises subjecting polyether-polyol(A) represented by the formula of HO- GBP (CH2)40|n- GBP (CR1R2)pO|q-H and having an average molecular weight of 500 to 4,500 to selective fractionation extraction using an aqueous solution(C) containing 15-70 wt% of sulfuric acid at a temperature from room temperature to 100 deg.C so as to obtain a low-molecular weight fraction, wherein the amount and concentration of the aqueous sulfuric acid solution based on those of the total organic layer are determined according to the molecular weight and molecular weight distribution of the target polyether-polyol to be extracted. In the above formula, R1 and R2 ae the same or different and each represents H or a linear or branched C1-C5 alkyl, n is a positive integer, p is an integer of 1-8, and q is 0 or a positive integer.

Description

technical field [0001] The invention relates to a preparation method of polyether polyol with narrow molecular weight distribution. The method is realized by controlling the molecular weight distribution of polyether polyol with tetrahydrofuran unit produced during tetrahydrofuran polymerization or tetrahydrofuran and other cyclic ether copolymerization process. Polyether polyols with tetrahydrofuran units have excellent elasticity and low-temperature properties, and have good hydrolysis resistance in polyurethane elastic fibers, polyurethane elastomers, polyether-polyester elastomers, and polyurethane-containing elastic coatings. It is a chemical A very important substance in the industrial field. Background technique [0002] In general, common polyether polyols prepared by cationic polymerization such as tetrahydrofuran polymerization or tetrahydrofuran copolymerization with other cyclic ethers have a broad molecular weight distribution. However, it is known that when po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/48C08G65/20C08G65/30
CPCC08G65/30C08G65/20C08G18/48
Inventor 冈部宪昭中冈弘吏兼平郁彦
Owner HODOGOYA CHEMICAL CO LTD