Method for preparing polyester ether polyol

A technology of polyester ether polyol and polyester polyol, applied in the field of preparation of polyester ether polyol, can solve the problems of high price of polyether polyol, high viscosity of polyester and high price

Inactive Publication Date: 2015-09-30
BEIJING ACAD OF BUILDING ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantages of polyester rigid foam are high strength, fine foam cells, low thermal conductivity, good adhesion and low price, but the polyester itself has a high viscosity and is inconvenient to operate, and the foam obtained from polyester is hydrolytically stable. poor sex
Polyether ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1) Add 218g (1mol) of pyromellitic anhydride, 212g (2mol) of diethylene glycol and potassium fluotitanate (0.43g) into a four-necked flask in sequence, and slowly raise the temperature to 120-140°C. Stop the reaction when the acid value of the product is less than or equal to 1.5 mg KOH / g; cool to below 90°C and filter out the material to obtain the pyromellitic acid polyester polyol.

[0017] 2) Add 400g of pyromellitic acid polyester polyol and 0.04g of dimethylamine into the polyether reaction kettle, reduce the pressure, gradually put 400g of propylene oxide into the kettle, and slowly raise the temperature to 100℃~130℃, and the pressure in the kettle is 0.07 ~0.4MPa, under this temperature and pressure, react for 3 hours, then vacuumize, wait until the temperature drops below 90°C and filter out the material, you can get pyromellitic acid polyester ether polyol (hydroxyl value 225mg KOH / g, Acid value 1.0mg KOH / g, moisture 0.03%).

Embodiment 2

[0019] 1) Add 218g (1mol) of pyromellitic anhydride, 318g (3mol) of diethylene glycol and dibutyltin oxide (0.5g) into a four-necked flask in sequence, and slowly raise the temperature to 120-140°C. Stop the reaction when the acid value of the product is less than or equal to 1.5 mg KOH / g; cool to below 90°C and filter out the material to obtain the pyromellitic acid polyester polyol.

[0020] 2) Add 400g of pyromellitic acid polyester polyol and 0.06g of trimethylamine into the polyether reaction kettle, reduce the pressure, gradually put 300g of propylene oxide into the kettle, and slowly raise the temperature to 100℃~130℃, and the pressure in the kettle is 0.07~ 0.4MPa, under this temperature and pressure, react for 3.5h, then evacuate, wait until the temperature drops below 90°C and filter out the material, you can get pyromellitic acid polyester ether polyol (hydroxyl value 205mg KOH / g, Acid value 1.2mg KOH / g, moisture 0.025%).

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PUM

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Abstract

The invention belongs to the technical field of chemical synthesis and particularly relates to a method for preparing polyester ether polyol. According to the method, pyromellitic dianhydride and dihydric alcohol serve as main raw materials, and through esterification reactions and etherification reactions, the polyester ether polyol is prepared out. The preparation method comprises the following steps: 1 putting the pyromellitic dianhydride, micromolecule dihydric alcohol and catalyst into a polyester reaction bottle, adding N[2] for production, and heating to the 120 DEG C to 140 DEG C. When product acid value is less than or equal to 1.5 mg KOH/g, stopping the reaction; cooling to be lower than 90 DEG C, conducting filter pressing, discharging materials, and obtaining pyromellitic acid polyester polyol. 2 putting the pyromellitic acid polyester polyol and amine catalyst into a polyether reaction still, and reducing pressure; putting epoxypropane into the reaction still, heating to 100 DEG C to 130 DEG C slowly, keeping the pressure inside the still to be within 0.07 MPa to 0.4 MPa, reacting for 1 h-4 h under the temperature and the pressure, conducting vacuuming, when the temperature lowers to be less than 90 DEG C, conducting filter pressing, discharging materials, and obtaining pyromellitic acid polyester ether polyol.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of polyester ether polyol. Background technique [0002] Polyester polyol and polyether polyol are important components of polyurethane foam. Polyester polyol is prepared by reacting dibasic acid or anhydride with diol or polyol. Polyether polyol is based on ethylene oxide, Epoxy compounds such as propylene oxide are polymerized monomers, oligomer polyols synthesized by ring-opening homopolymerization and copolymerization with polyhydroxyl and amine compounds as initiators. The advantages of polyester rigid foam are high strength, fine foam cells, low thermal conductivity, good adhesion and low price, but the polyester itself has a high viscosity and is inconvenient to operate, and the foam obtained from polyester is hydrolytically stable. Poor sex. Polyether polyols have good hydrolysis stability and good compatibility with other add...

Claims

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Application Information

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IPC IPC(8): C08G65/28
Inventor 王万金贺奎董全霄樊勇朱宁夏义兵吴敬朋王靖贾方方赖振峰郭现龙
Owner BEIJING ACAD OF BUILDING ENG
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