Preparation method of high-storage-stability polyester-type polyurethane prepolymer

A polyester polyurethane, storage-stable technology, applied in the field of polyurethane prepolymer preparation, can solve the problems of unstable performance of polyester polyurethane prepolymer and the like

Active Publication Date: 2011-08-24
SHANXI CHEM RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The object of the present invention is to provide a kind of preparation method of the polyester polyurethane prepolymer of storage stability for the unstable performance of existing polyester polyurethane prepolymer, make NCO% in the polyester polyurethane prepolymer that makes The content change is less than 0.2%, and the product is stable in storage

Method used

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  • Preparation method of high-storage-stability polyester-type polyurethane prepolymer
  • Preparation method of high-storage-stability polyester-type polyurethane prepolymer
  • Preparation method of high-storage-stability polyester-type polyurethane prepolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Add 1000 grams of polyester polyol ODX-218 (Yantai Huada Chemical Industry Co., Ltd., Mn=2000) and 0.015 grams of metal ion complexing agent triethylamine into a mixing device, thermometer and dry nitrogen protection In the reactor of the device, heat and stir to raise the temperature. When the temperature rises to 120°C, stop nitrogen flow, start vacuum dehydration, vacuum degree 0.084MPa, dehydrate for 2 hours, then cool down to 50°C for use.

[0029] 2) The NCO% value of the polyurethane prepolymer is designed to be 3.7, and 177.1 grams of the required 2,4-toluene diisocyanate are added to a reactor equipped with a stirring device, a feed port, a thermometer and a dry nitrogen protection device, at 0.5 Add the materials in step 1) in 5 times within one hour, keep the reaction temperature at 50°C, react for 0.5 hours, heat up to 85°C at a heating rate of 10°C / 20 minutes, and maintain the reaction for 2 hours.

[0030] 3) Add 0.006 gram of polymerization inhibitor p...

Embodiment 2

[0039] 1) Add 1000 grams of polyester polyol ODX-150 (Yantai Huada Chemical Industry Co., Ltd., Mn=1500) and 0.01 gram of metal ion complexing agent triisopropanolamine into a mixing device, thermometer and dry nitrogen In the reactor of the protection device, heat and stir to raise the temperature. When the temperature rises to 110°C, stop nitrogen flow, start vacuum dehydration, vacuum degree 0.086MPa, dehydrate for 2 hours, then cool down to 45°C for use.

[0040]2) The NCO% value of the polyurethane prepolymer is designed to be 4.8, and 239 grams of the required 2,4-toluene diisocyanate are added to a reactor equipped with a stirring device, a feed port, a thermometer and a dry nitrogen protection device, at 0.5 Add the materials in step 1) in 5 times within one hour, keep the reaction temperature at 45°C, react for 0.5 hours, heat up to 82°C at a heating rate of 10°C / 20 minutes, and maintain the reaction for 2 hours.

[0041] 3) Add 0.01 gram of polymerization inhibitor b...

Embodiment 3

[0048] 1) 1000 grams of polyester polyol CMA-1024 (Yantai Huada Chemical Industry Co., Ltd., Mn=1000) and 0.008 grams of metal ion complexing agent disodium diamine tetraacetate are added to a mixing device, thermometer and In the reactor of the dry nitrogen protection device, heat and stir to raise the temperature. When the temperature rises to 115°C, stop nitrogen flow, start vacuum dehydration, vacuum degree 0.088MPa, dehydrate for 2 hours, then cool down to 40°C for use.

[0049] 2) The NCO% value of the polyurethane prepolymer is designed to be 5.1, and 312.5 grams of the required 2,4-toluene diisocyanate are added to a reactor equipped with a stirring device, a feed port, a thermometer and a dry nitrogen protection device, at 0.5 Add the materials in step 1) in 5 times within one hour, keep the reaction temperature at 40°C, react for 0.5 hours, heat up to 80°C at a heating rate of 10°C / 20 minutes, and maintain the reaction for 2 hours.

[0050] 3) Add 0.015 grams of poly...

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Abstract

The invention relates to a preparation method of a high-storage-stability polyester-type polyurethane prepolymer, which comprises the following steps: adding a nitrogen-containing metallic ion complexing agent into a hydroxyl-terminated low-polymer polyester polyol; dewatering at 95-130 DEG C under the vacuum degree of 0.08-0.09 MPa for 2 hours; cooling to 30-55 DEG C, mixing with 2,4-toluene diisocyanate, and reacting at controlled temperature of 30-65 DEG C for 0.5 hour; heating to 70-95 DEG C, and keeping the reaction for 2 hours; adding a polymerization inhibitor, and deaerating at controlled temperature of 70-95 DEG C under the pressure of 0.08-0.09 MPa for 0.5 hour to obtain the high-storage-stability polyester-type polyurethane prepolymer; and after measuring that the percentage ofNCO (isocyanate-group) in the prepolymer is equivalent to a set value, cooling, charging nitrogen, and storing in a closed environment. The change rate of the percentage of NCO in the obtained polyester-type polyurethane prepolymer is less than 0.2%, and thus, the polyester-type polyurethane prepolymer can be stored stably.

Description

technical field [0001] The invention relates to a preparation method of a polyurethane prepolymer, in particular to a preparation method of a storage-stable polyurethane prepolymer. Background technique [0002] Polyurethane prepolymers refer to adducts made by reacting hydroxyl-containing compounds with isocyanate monomers. The isocyanate group has high reactivity, and it is very easy to react with the moisture in the air and the impurities containing active hydrogen in the system, which will increase the viscosity of the prepolymer or even gel. Therefore, storage stability is one of the important technical indicators of polyurethane prepolymers. [0003] In order to prolong the shelf life of prepolymers, methods such as reducing moisture, removing harmful impurities, and controlling unnecessary reactions have been used. For example: German patents 2036872 and 2036873 require that the residual moisture content of hydroxyl compounds <0.1%, preferably <0.05%, and use ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/76C08G18/42C08G18/10
Inventor 贾林才孙勇洛桂娥刘凉冰原志峰刘红梅张福兵陆建伟乔玉同孙奉瑞
Owner SHANXI CHEM RES INST
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