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Unsaturated polycarbonate diol and preparation method thereof

A polycarbonate diol, unsaturated technology, applied in the field of polymer materials, to achieve the effect of broadening the application range, increasing the cross-linking density and hardness, and increasing the cross-linking density

Active Publication Date: 2014-09-10
新丰博兴聚合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, on the basis of making full use of the high flexibility and high toughness of the existing polycarbonate urethane acrylate, if the existing polycarbonate urethane acrylate can be modified through molecular design, it may meet the needs of new applications

Method used

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  • Unsaturated polycarbonate diol and preparation method thereof
  • Unsaturated polycarbonate diol and preparation method thereof
  • Unsaturated polycarbonate diol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～9

[0042] Example 1 ~ 9 Synthesis of unsaturated polycarbonate diols

[0043] Add 3.0 mol (354.3 g) purified diethyl carbonate, 3.5 mol (317.8 g) Z-2-butene-1,4-diol ( Purity 97%), 7.2 g 2,6-di-tert-butylphenol, some catalysts, nitrogen gas, heated to 135°C to boil, when the thermometer at the top of the reflux tube indicated about 81°C, ethanol began to distill out, the raw material diethyl carbonate The ester is in a reflux state, and when the distillation of ethanol stops, the temperature of the reaction bottle is raised to 155°C, and a negative pressure is applied to control the pressure at 8-12 mmHg, and the reaction is continued for 1 hour. The reaction was stopped, cooled, and samples were taken for GPC molecular weight determination and infrared spectroscopic testing. The infrared spectrum of embodiment 1~9 shows product at 1625 cm -1 There is a C=C double bond absorption peak at 3031 cm -1 There is an unsaturated C-H bond absorption peak.

[0044] Table 1:

[004...

Embodiment 10

[0046] The synthesis of embodiment 10 unsaturated polycarbonate diols

[0047] Same as Example 9, but 3.0 mol (354.3 g) of purified diethyl carbonate is replaced by 3.0 mol (270.3 g) of purified dimethyl carbonate, the reflux reaction temperature is controlled at 95°C, and the distillation head thermometer reaches 67°C Around the time, methanol began to distill out. The raw material dimethyl carbonate is in a reflux state. When the distillation of methanol stops, the temperature of the reaction bottle is raised to 115° C., and a negative pressure is applied to control the pressure at 8-12 mmHg, and the reaction is continued for 1 hour. The reaction was stopped, cooled, and samples were taken for GPC molecular weight determination and infrared spectroscopic testing. Infrared spectrum showed that the product was at 1625 cm -1 There is a C=C double bond absorption peak at 3031 cm -1 There is an unsaturated C-H bond absorption peak. The reaction time of distilling off ethano...

Embodiment 11～19

[0048] Example 11 ~ 19 Synthesis of unsaturated polycarbonate diols

[0049] Add 3.0 mol (354.3 g) of purified diethyl carbonate and 3.5 mol of olefin diol (oligomer diol is measured by hydroxyl value) into a three-necked flask equipped with a reflux condenser and connected to a distillation head, quantitatively 2, 6-di-tert-butylphenol, lithium iron hexafluorophosphate as a catalyst, nitrogen gas, heated to 135 ° C to boil, when the thermometer at the top of the reflux tube indicates about 81 ° C, ethanol begins to distill, and the raw material diethyl carbonate The ester is in a reflux state, and when the distillation of ethanol stops, the temperature of the reaction bottle is raised to 155°C, and a negative pressure is applied to control the pressure at 8-12 mmHg, and the reaction is continued for 1 hour. The reaction was stopped, cooled, and samples were taken for GPC molecular weight determination and infrared spectroscopic testing. The infrared spectrum of embodimen...

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Abstract

The invention relates to the field of polymer materials, particularly to unsaturated polycarbonate diol and a preparation method thereof. The unsaturated polycarbonate diol is prepared from one or more of aliphatic diols and carbonyldioxy dialkyl ester under ester exchange catalyst condition through an ester exchange reaction; the number-average molecular weight of the unsaturated polycarbonate diol is 300-8000. According to the invention, the defects that saturated polycarbonate diol in the prior art is only subjected to one-off cross-linking polymerization are overcome and the unsaturated polycarbonate diol and the preparation method thereof are provided; properties of the unsaturated polycarbonate diol such as tensile property, water resistance, crosslinking density and hardness are increased so that the application range of polycarbonate diol materials is broadened.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to an unsaturated polycarbonate diol and a preparation method thereof. Background technique [0002] Diols with a certain molecular weight are important raw materials for the synthesis of polyurethane materials. Traditional diols mainly include polyether diols and polyester diols, which have good reactivity with isocyanates. However, polyurethane materials formed by polyethers such as polyethylene glycol, polypropylene glycol, and polytetramethylene glycol are not good enough in water resistance, heat resistance, chemical resistance, solvent resistance, etc., or even poor; Although the hydrolysis resistance has been improved, it is still not good enough, and others such as solvent resistance, chemical resistance, and antibacterial properties are not at a good level. The emerging aliphatic polycarbonate diol is different from the traditional aromatic polycarbonate. It is a kind of o...

Claims

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Application Information

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IPC IPC(8): C08G64/30C08G64/02C07C69/96C07C68/06C08G18/67C09D175/14
Inventor 庞来兴
Owner 新丰博兴聚合材料有限公司