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Aliphatic polycarbonate diol preparation method, catalyst and preparation method thereof

A polycarbonate two, aliphatic technology, applied in the field of magnetic heterogeneous catalysts, can solve problems such as catalyst separation difficulties, and achieve the effects of convenient separation, easy-to-obtain raw materials, and simple methods

Active Publication Date: 2019-01-29
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the purposes of the present invention is to: solve the problem of catalyst separation difficulties in the synthesis of PCDLs by transesterification, provide a magnetic solid base as a heterogeneous catalyst, the separation of the catalyst is fast and convenient

Method used

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  • Aliphatic polycarbonate diol preparation method, catalyst and preparation method thereof
  • Aliphatic polycarbonate diol preparation method, catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 10.17g MgCl 2 ·6H 2 O and 6.95 g FeSO 4 ·7H 2 O was dissolved in 250ml of distilled water, recorded as solution A; 10.08g of Na 2 C 2 o 4 Dissolve in 250ml of distilled water and record it as solution B. Add solution B to solution A dropwise using a constant flow pump at room temperature. After the dropwise addition, the obtained precipitate was filtered, washed, and then dried in an oven at 60° C. for 12 hours to obtain a Mg-Fe composite oxide precursor. Put the precursor in a muffle furnace, set the temperature rise program of the muffle furnace, raise the temperature in the muffle furnace to 400°C at a rate of 10°C / min, and bake at 400°C for 2h to obtain magnetic Mg- Fe oxides.

[0024] 0.2g KF·2H 2 O was dissolved in 3ml of methanol, 1g of magnetic Mg-Fe oxide was added, after ultrasonic dispersion was uniform, it was left to stand at room temperature for 6h, and then the system was placed in a 100°C oven to dry for 12h, and then placed in a muffle furnace ...

Embodiment 2

[0026] 12.82g Mg(NO 3 ) 2 ·6H 2 O and 4.97 g FeCl 2 4H 2O was dissolved in 250ml distilled water, recorded as solution A; 13.82g K 2 C 2 o 4 ·H 2 O was dissolved in 250ml of distilled water, which was recorded as solution B. Add solution B to solution A dropwise using a constant flow pump at room temperature. The precipitate was filtered, washed, and dried in an oven at 60° C. for 10 h to obtain a Mg—Fe oxide precursor. Put the precursor in a muffle furnace, raise the temperature to 400°C at a rate of 25°C / min, and bake at this temperature for 2h to obtain magnetic Mg-Fe oxides.

[0027] 0.2g KF·2H 2 O was dissolved in 3ml of distilled water, 1g of Mg-Fe composite oxide carrier was added, after ultrasonic dispersion, it was left at room temperature for 6h, dried in an oven at 100°C for one night, then placed in a muffle furnace, and roasted at 500°C for 2h to obtain KF / xMgO·Mg 2 Fe 2 o 4 Magnetic solid base catalyst.

Embodiment 3

[0028] Embodiment 3: The difference between this embodiment and Embodiment 1 is that in this embodiment, 0.5g KF·2H 2 O was dissolved in 4ml of distilled water, and 1g of Mg-Fe composite oxide carrier was added, and the rest of the steps were the same as in Example 1.

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Abstract

The invention discloses a magnetic solid base catalyst for preparing aliphatic polycarbonate diol, wherein the magnetic solid base catalyst comprises magnetic Mg-Fe oxide and KF loaded on the magneticMg-Fe oxide, wherein the mass fraction of KF in the magnetic solid base catalyst is 5 wt%-40 wt%. The magnetic solid base catalyst comprises the following preparation steps: (1) taking magnesium salt, ferric salt and alkali as raw materials, preparing precursors by adopting a coprecipitation method, placing the prepared precursors in a muffle furnace, heating to 300-500 DEG C at the heating speedof 1-25 DEG C / min, carrying out thermal-insulation at the temperature for 1-4 hours to obtain the magnetic Mg-Fe oxide, wherein that amount ratio of the magnesium salt to the iron salt is 1: 5-5: 1;(2) dissolving KF.2H2O in a solvent, and adding the magnetic Mg-Fe oxide prepared in the step (1), performing uniform ultrasonic dispersing, standing at room temperature for 6 hours, drying in an oven, and placing in the muffle furnace, wherein that temperature is 400 DEG C, roasting at 400-600 DEG C for 0.5-4 hours, so as to obtain the magnetic solid base catalyst.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a preparation method of aliphatic polycarbonate diol and a magnetic heterogeneous catalyst used in the method. Background technique [0002] Polycarbonate diols (PCDLs) are polymers with hydroxyl (-OH) at the end of the molecule and repeating units of aliphatic alkylene and carbonate groups (-OCOO-) in the main chain of the molecule. It is a high-performance special polyol . Aliphatic polycarbonate diols with a molecular weight of 500-3000 g / mol are considered to be the polyols with the best performance at present. Its important downstream product - polycarbonate polyurethane material, can be widely used in construction, metallurgy, chemical industry, electromechanical and medical and health fields. Compared with traditional polyether polyurethanes and polyester polyurethanes, polycarbonate polyurethanes are improved in terms of heat resistance, weather re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/30C08G64/02
CPCC08G64/0208C08G64/305
Inventor 杨先贵宋孟璐王公应
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI