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Aliphatic polycarbonate dibasic alcohol and preparation method thereof

A technology of aliphatic diol and polycarbonate diol, which is applied in the field of aliphatic polycarbonate diol and its preparation, and achieves the effects of easy impurity removal, good effect, and no solvent needed

Active Publication Date: 2016-06-22
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the technical problems of the existing aliphatic polycarbonate diol preparation method, to provide a kind of preparation method of aliphatic polycarbonate diol

Method used

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  • Aliphatic polycarbonate dibasic alcohol and preparation method thereof
  • Aliphatic polycarbonate dibasic alcohol and preparation method thereof
  • Aliphatic polycarbonate dibasic alcohol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 10.2g (100mmol) of polymethylethylene carbonate, 0.21g of sodium carbonate (2%), and 2.51g (33mmol) of 1,2-propanediol into a heating and stirring system, temperature measuring system and reflux system inside the reactor. Repeatedly evacuate and ventilate the nitrogen to remove the air in the reactor (at least 3 times), and raise the temperature to 180°C at normal pressure under the nitrogen atmosphere, and react for 1h. Nitrogen gas is passed to allow the product to cool to obtain the primary product of polymethylethylene carbonate diol. The obtained primary product is a slightly yellow viscous liquid at room temperature, which can be washed 3 times with water, and the by-products can be removed after soaking, and the color turns white. Then azeotropic distillation with toluene removes the water therein, and the polymethylethylene carbonate diol is obtained after drying.

[0034] Product parameters:

[0035]

Embodiment 2

[0037] Add 10.2g (100mmol) of polymethylethylene carbonate, 53mg of sodium carbonate (0.5%), and 1.50g (16.67mmol) of 1,4-butanediol into a heating and stirring system, temperature measuring system and reflux in the reactor of the system. Repeatedly evacuate and ventilate the nitrogen to remove the air in the reactor (at least 3 times), raise the temperature to 150°C at normal pressure under nitrogen atmosphere, and react for 3 hours. Nitrogen gas is passed to allow the product to cool to obtain the primary product of polymethylethylene carbonate diol. The obtained primary product is a slightly yellow viscous liquid at room temperature, which can be washed 3 times with water, and the by-products can be removed after soaking, and the color turns white. Then azeotropic distillation with toluene removes the water therein, and the polymethylethylene carbonate diol is obtained after drying.

[0038] Product parameters:

[0039]

Embodiment 3

[0041] Add 10.2g (100mmol) of polymethylethylene carbonate, 0.42g of sodium bicarbonate (5.0%), and 11.80g (100mmol) of 1,6-hexanediol into a heating and stirring system, temperature measuring system and In the reactor of the reflux system. Repeatedly evacuate the nitrogen to remove the air in the reactor (at least 3 times), raise the temperature to 100°C under the nitrogen atmosphere, and react for 20h. Nitrogen gas is allowed to cool the product to obtain polymethylethylene carbonate diol. The obtained primary product is a slightly yellow viscous liquid at room temperature, which can be washed 3 times with water, and the by-products can be removed after soaking, and the color turns white. Then azeotropic distillation with toluene removes the water therein, and the polymethylethylene carbonate diol is obtained after drying.

[0042] Product parameters:

[0043]

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Abstract

The invention relates to the technical field of polymer materials, and discloses an aliphatic polycarbonate dibasic alcohol and a preparation method thereof. The preparation method of the aliphatic polycarbonate dibasic alcohol comprises the following steps: carrying out ester exchange reaction on polymethylethylene carbonate and an aliphatic dibasic alcohol under the condition of a catalyst, and removing impurities, wherein the molecular weight of the polymethylethylene carbonate is greater than 10000Da. The molar weight of the aliphatic dibasic alcohol accounts for 15-100% of that of the polymethylethylene carbonate. The catalyst accounts for 0.01-5% of the molar weight of the polymethylethylene carbonate. The ester exchange reaction is performed by heating to 80-180 DEG C in an inert gas atmosphere and refluxing for 1-30 hours. The invention provides a method for preparing low-molecular-weight aliphatic polycarbonate dibasic alcohol from high-molecular-weight polycarbonate, and widens the applicability of the high-molecular-weight polycarbonate. The molecular weight of the aliphatic polycarbonate dibasic alcohol and the hydroxy functional group degree can be adjusted according to needs, and the primary product of the aliphatic polycarbonate dibasic alcohol is easy for impurity removal.

Description

technical field [0001] The present invention relates to the technical field of polymer materials, and more specifically, relates to an aliphatic polycarbonate diol and a preparation method thereof. Background technique [0002] Polyurethane is a polymer compound obtained by polycondensation reaction of isocyanate and polyol. The raw materials for the main soft segment of polyurethane resins produced on an industrial scale can be classified into ethers represented by polytetramethylene glycol, polyester diols represented by adipate, and polyols represented by polycaprolactone. Polycarbonates represented by lactones and polycarbonate diols. [0003] Among them, aliphatic polycarbonate diol (APC) is a compound with multiple carbonate groups in the molecule and terminated by hydroxyl groups. The structural formula is as follows: . Due to the greater flexibility of its molecular chain, it can be used as a raw material for the synthesis of a new generation of polycarbonate pol...

Claims

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Application Information

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IPC IPC(8): C08G64/38C08G64/02C08G18/44
CPCC08G18/44C08G64/0208C08G64/38
Inventor 孟跃中罗伟铿王拴紧肖敏韩东梅
Owner SUN YAT SEN UNIV
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