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Branching polycarbonate polyhydric alcohol, preparation method and application thereof

A technology of polycarbonate diol and polycarbonate, which is applied in the field of polymers, can solve the problems of shortened solid curing time, weather resistance, high content of low-molecular-weight diols, and wide molecular weight distribution of products, so as to achieve easy control of molecular weight, The effect of high activity and shortened curing time

Active Publication Date: 2019-03-01
JIANGSU RUIYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst selection for the transesterification reaction is the most critical. The currently used catalysts have disadvantages such as low boiling point, volatile during the reaction process, unfavorable for decompression and compression polymerization, and low catalytic activity.
In addition, the current process is to azeotrope excess dimethyl carbonate and by-product methanol (azeotropic point 64°C) to bring out methanol. Due to the low reaction temperature and the difficulty in precise control of the composition of the azeotrope, it is difficult to measure the reactants, resulting in polycondensation of the product. High content of low-molecular-weight diols in carbonate diol, wide product molecular weight distribution, difficult to control molecular weight
Further, the mechanical properties, water resistance, and softness of the existing polyurethane still need to be further improved, especially the curing time needs to be further shortened, and the weather resistance needs to be further improved

Method used

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  • Branching polycarbonate polyhydric alcohol, preparation method and application thereof
  • Branching polycarbonate polyhydric alcohol, preparation method and application thereof
  • Branching polycarbonate polyhydric alcohol, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A branched polycarbonate polyol with a number average molecular weight of 3500, a molecular weight distribution of 2.87 and a hydroxyl value of 128.

[0037] The preparation method of above-mentioned branched polycarbonate polyol may further comprise the steps:

[0038] (1) Synthesis of intermediate low molecular weight polycarbonate containing dimethyl ester

[0039]Butanediol (9.00g, 100mmol) and dimethyl carbonate (18.00g, 200mmol) were added to a 250mL reactor, the temperature was raised to 85°C, oxygen was exhausted during reflux, and then the catalyst pentamethyldiethylenetriamine was placed online (0.00086g, 0.05mmol) was added to the reaction kettle, and the reaction was stirred. The stirred kettle was equipped with a rectification device to separate dimethyl carbonate and methanol. The dimethyl carbonate was refluxed to the reaction to continue to participate in the reaction, and the by-product methanol was removed. Gas chromatography Track the butanediol reac...

Embodiment 2

[0043] A kind of synthesis of branched polycarbonate polyol:

[0044] The difference from Example 1 is that the molecular weight of the intermediate polycarbonate containing dimethyl ester at the end group is 500, the molecular weight of the branched polycarbonate polyol is 4600, the molecular weight distribution is 2.95, and the hydroxyl value is 135.

[0045] Without changing other conditions of Example 1, in step (1), the mass ratio of butanediol (9.00g, 100mmol) and dimethyl carbonate (15.30g, 170mmol) in the preparation process is 1: 1.7, the amount of catalyst is 0.05mmol, and the operation process remains unchanged, and the polycarbonate containing dimethyl ester in the end group is successfully prepared, and the nuclear magnetic calculation molecular weight is 500, and the quality is 18.7g, and the yield is 94.9%; in step (2), Add butanediol (3.9g, 44mmol) and glycerol (1.7g, 18mmol), operation process is constant, the number average molecular weight that draws polymer...

Embodiment 3

[0047] A kind of synthesis of branched polycarbonate polyol:

[0048] The difference from Example 1 is that the molecular weight of the intermediate polycarbonate containing dimethyl ester at the end group is 700, the molecular weight of the branched polycarbonate polyol is 5500, the molecular weight distribution is 3.15, and the hydroxyl value is 140.

[0049] Under the situation of not changing other conditions of Example 1, in step (1), the mass ratio of butanediol (9.00g, 100mmol) and dimethyl carbonate (13.50g, 150mmol) in the preparation process is 1: 1.5, the amount of catalyst is 0.05mmol, the operation process is unchanged, successfully prepared polycarbonate containing dimethyl ester at the end group, the molecular weight is 700, the quality is 14.5g, and the yield is 97.2%; in step (2), add butanediol Alcohol (2.0g, 22mmol) and glycerol (1.7g, 18mmol), operating process is constant, and the number-average molecular weight that draws polymer by gel permeation chromat...

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Abstract

The invention discloses a branching polycarbonate polyhydric alcohol, a preparation method and an application thereof. The structural formula of the branching polycarbonate polyhydric alcohol is as follows. The preparation method for the branching polycarbonate polyhydric alcohol comprises the following steps in turn: 1) reacting dimethyl carbonate and dihydric alcohol under the catalytic effect of pentamethyl diethylenetriamine, thereby acquiring an intermediate polycarbonate containing dimethyl in end group; 2) adding dihydric alcohol and polyhydric alcohol into the material acquired in thestep 1) and reacting, thereby acquiring the branching polycarbonate polyhydric alcohol, wherein the polyhydric alcohol is trihydric alcohol to pentahydric alcohol. According to the invention, a two-step process is adopted and an efficient catalyst is selected for accurately controlling molecular weight of polymer and preparing the branching polycarbonate polyhydric alcohol.

Description

technical field [0001] The invention relates to the field of macromolecules, and is a polyester polyol for polyurethane, in particular to a branched polycarbonate polyol, its preparation method and its application. Background technique [0002] The flexible segment of synthetic polyurethane resin is oligomer polyol, which can improve the flexibility and toughness of polyurethane elastomer. There are many types of oligomer polyols, such as polyether polyols, polyester polyols, polycarbonate polyols, etc. At present, in the field of polyurethane synthesis, polyether polyols and polyester polyols are the two most commonly used in consideration of factors such as polyol production cost and performance. However, polyurethane materials composed of polyester polyols usually have the characteristics of good mechanical and mechanical properties, oil resistance, and excellent abrasion resistance. Poor performance, poor hydrolysis resistance, and high production costs hinder the appl...

Claims

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Application Information

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IPC IPC(8): C08G64/30C08G18/44
CPCC08G18/44C08G64/305
Inventor 薛小强彭枝忠孙佳悦薛志强
Owner JIANGSU RUIYANG CHEM
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