Method for preparing adipic acid polyester polyol by utilizing recycled alcohol

A technology for adipic acid polyester and alcohol recovery, which is applied in the direction of chemical recovery, can solve the problems of difficult water removal, refining and purification costs, high energy consumption, and large consumption, and achieves low production costs, high heating efficiency, The effect of environmentally friendly and low energy consumption reuse

Active Publication Date: 2014-03-19
JIANGSU YINGTIAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1,2-propanediol is used as a cleaning agent in a large amount, and the water brought in after cleaning is difficult to remove, and its refining and purification costs and energy consumption are relatively high

Method used

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  • Method for preparing adipic acid polyester polyol by utilizing recycled alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1): Put 50Kg of recycled solar wafer cutting fluid (hydroxyl value 500mg KOH / g), 50Kg of recycled 1,2-propanediol (content 95%), 100Kg of adipic acid and 25g of monobutyltin oxide into the polyester reaction at one time in the kettle

[0027] 2): Using high temperature and high pressure steam heating method, after the temperature rises to 130°C, N 2 , continue to heat up to 142°C, and react for 2h;

[0028] 3): pass into N 2 Use as protective gas and keep it uninterrupted, continue to heat up to 180°C, and react for 2 hours;

[0029] 4): heat up to 225°C, keep warm for 2 hours;

[0030] 5): Start vacuuming, the pressure and temperature are finally stabilized at -0.09MPa and 225°C, and the reaction is stopped when the acid value of the product is ≤0.9mg KOH / g.

[0031] 6): Cool to below 80°C and filter the material to obtain viscous transparent adipic acid polyester polyol (hydroxyl value 75mg KOH / g, acid value 0.8mg KOH / g, moisture 0.03%, chroma 230 Hazen).

Embodiment 2

[0033] 1): Put 68Kg of recycled solar wafer cutting fluid (hydroxyl value 598mg KOH / g), 35Kg of recycled 1,2-propanediol (90% content), 100Kg of adipic acid and 61g of monobutyltin oxide into polyester at one time In the reactor;

[0034] 2): Using high temperature and high pressure steam heating method, after the temperature rises to 130°C, N 2 , continue to heat up to 145°C, and react for 1h;

[0035] 3): pass into N 2 Use as protective gas and keep it uninterrupted, continue to heat up to 185°C, and react for 1h;

[0036] 4): Heat up to 230°C and keep warm for 1 hour;

[0037] 5): Start vacuuming, the pressure and temperature are finally stabilized at -0.095MPa and 225°C, and the reaction is stopped when the acid value of the product is ≤0.9mg KOH / g.

[0038] 6): Cool down to below 80°C and press filter to get viscous transparent adipic acid polyester polyol (hydroxyl value 40mg KOH / g, acid value 0.7mg KOH / g, moisture 0.02%, chroma 270 Hazen).

Embodiment 3

[0040] 1): Add 80Kg of recycled solar wafer cutting fluid (hydroxyl value 750mg KOH / g), 30Kg of recycled 1,2-propanediol (content 90%), 100Kg of adipic acid and 32g of monobutyltin oxide into polyester at one time In the reactor;

[0041] 2): Using high temperature and high pressure steam heating method, after the temperature rises to 130°C, N 2 , continue to heat up to 144°C, and react for 1.5h;

[0042] 3): pass into N 2 Use as protective gas and keep it uninterrupted, continue to heat up to 182°C, and react for 1.5h;

[0043] 4): heat up to 228°C, keep warm for 1.5h;

[0044] 5): Start vacuuming, the pressure and temperature are finally stabilized at -0.095MPa and 226°C, and the reaction is stopped when the acid value of the product is ≤0.9mg KOH / g.

[0045] 6): Cool down to below 80°C and filter the material to obtain viscous transparent adipic acid polyester polyol (hydroxyl value 126mg KOH / g, acid value 0.8mg KOH / g, moisture 0.03%, chroma 300 Hazen).

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Abstract

The invention discloses a method for preparing adipic acid polyester polyol by utilizing recycled alcohol. The method comprises the following steps: 1) putting recovered alcohol, adipic acid, a catalyst and the like into a polyester reaction kettle at a time; 2) when the temperature rises to 130 DEG C, introducing N2, continuing heating up to 142-145 DEG C, and carrying out a reaction for 1-2 h; 3) continuing heating up to 180-185 DEG C, and carrying out the reaction for 1-2 h; 4) heating up to 225-230 DEG C, and holding for 1-2 h; 5) vacuumizing, and when the product acid value is not more than 0.9 mg KOH / g, stopping the reaction; and 6) cooling to below 80 DEG C, carrying out filter-pressing material discharge, and thus obtaining the adipic acid polyester polyol. With adopting of the above scheme, the adipic acid polyester polyol is obtained; with utilization of the recycled low-molecular polyol, the method makes the best use of everything; and moreover, with adopting of the high-temperature high-pressure steam heating method, the method is more environmentally friendly and saves energy, has relatively low production cost, and allows the product to more have market competitive advantages.

Description

technical field [0001] The invention relates to the field of synthesis of hexanediol-based polyester polyols, in particular to a method for preparing adipic acid-based polyester polyols by utilizing recovered alcohol. Background technique [0002] Adipic acid polyester polyol is one of the important raw materials for the synthesis of polyurethane products. It is a chain-like compound that reacts with polyacids and polyols and ends with hydroxyl groups. It is widely used in adhesives, coatings, and shoe materials. , water-based polyurethane and synthetic leather and other fields. Polyester polyol is fully biodegradable and will not pollute the environment. It is one of the most in-depth research and most promising environmental protection materials for industrialization. [0003] Chinese patent CN201110301037.4 discloses a method for preparing a water-resistant and cold-resistant polyester polyol, which specifically relates to a method for preparing polyester polyol by react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/78C08G18/42
CPCY02P20/584
Inventor 杨水清罗伟蒋文俊陈玉龙王荣华
Owner JIANGSU YINGTIAN CHEM
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