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Preparation method of aqueous polyester polyol dispersoid

A dispersion and polyester technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve problems such as high resin acid value, increased VOC content, stability problems, etc., achieve high gloss, improve mechanical properties and durability High stability and high effect

Inactive Publication Date: 2010-09-08
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the coating stability prepared by this resin is not good
The reason is that in the resin synthesis reaction, when 5-SSIPA is polymerized with diols and dibasic carboxylic acids, the 5-SSIPA molecules tend to be at the end of the polyester chain, resulting in too high acid value of the resin, which causes stability problems
USP 5218042 discloses a new method for the synthesis of water-based polyester resins for this problem, that is: first react the neopentyl glycol NPG and 5-SSIPA of the formulation amount under catalyst conditions until the solution becomes clear, and then add the formulation amount The trimethylolpropane TMP, isophthalic acid IPA, and adipic acid AD continue to react to prepare water-based polyester resin. This method solves the problem of stability, but the process takes a long time and is added during the preparation of the dispersion. Added co-solvent, increased VOC content
Domestic patents related to realizing water-based polyester with sulfonate functional groups, such as CN 200510038276.X, CN03112011.3, CN 03112012.1, and CN 200610085553.7, all involve the technical field of fiber or polyester, and there is no disclosed method of using it in the preparation of water-based coatings. The Technology of Introducing Sulfonate Group to Realize Waterborne Polyester

Method used

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  • Preparation method of aqueous polyester polyol dispersoid
  • Preparation method of aqueous polyester polyol dispersoid
  • Preparation method of aqueous polyester polyol dispersoid

Examples

Experimental program
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Effect test

Embodiment 1

[0072] (1) Preparation of polyester intermediate: 81g neopentyl glycol, 70g isophthalic acid-5-sodium sulfonate, 0.17g Fascat 4100 and 20g deionized water are added to a mixture with stirring rod, condensing device, thermocouple and In a four-neck round-bottomed flask with a nitrogen inlet, pass nitrogen gas, raise the temperature to 90°C while stirring, and keep the temperature for half an hour. Then heat at 100-160°C for 2 hours, 160-200°C for 2 hours, heat at 210°C at a constant temperature until the acid value is less than 2mgKOH / g, then cool down, pour it into a mortar while it is hot, grind it to powder, and store it under dry conditions ;

[0073] (2) Preparation of polyester polyol aqueous dispersion: add the polyester intermediate 16.9g of embodiment 1 in the four-necked round-bottomed flask that has stirrer, condensation pipe, water trap, thermocouple and nitrogen inlet, Neopentyl glycol 43.6g, isophthalic acid 46.9g, trimethylolpropane 7.4g, and acid catalyst Fasca...

Embodiment 2

[0092] (1) Preparation of polyester intermediate: with the step (1) of embodiment 1;

[0093] (2) Preparation of polyester polyol aqueous dispersion: add the polyester intermediate prepared in step (1) in a four-necked round bottom flask with agitator, condenser, water separator, thermocouple and nitrogen inlet 13.5g, neopentyl glycol 34.8g, terephthalic acid 37.5g, trimethylolpropane 5.9g, and acid catalyst Fascat 41000.7g, and nitrogen was passed. Heat at 120°C, 140°C, and 160°C for 0.5 hour, 180°C for 1 hour, and raise the temperature to 220°C for constant temperature heating. When the solution became transparent, the temperature was lowered to 120°C, 28g of adipic acid was added, the temperature was slowly raised to 180°C, and the remaining 5.9g of trimethylolpropane was added. Slowly raise the temperature to 220°C and heat at a constant temperature until the acid value is less than 10mgKOH / g. Cool down the resin to 80°C, slowly add 120g of deionized water, stir and disp...

Embodiment 3

[0113] Embodiment 3: the preparation method of polyester polyol aqueous dispersion has the following steps:

[0114] (1) will have -SO 3 The dicarboxylic acid of the M group reacts with the dihydric alcohol to prepare the polyester intermediate: add -SO in the reactor 3 M-group dicarboxylic acid, glycol, catalyst, deionized water, introduce nitrogen and raise the temperature, control the reaction temperature 140 ° C ~ 160 ° C, the reaction time is about 9 hours; when the acid value of the mixed material in the reactor is 0.6, Stop the reaction to obtain a polyester intermediate; the amount of each component is: dibasic alcohol and -SO 3 The molar ratio of the dicarboxylic acid of the M group is 3:1, and the consumption of the catalyst is 0.6wt% of the total amount of alcohol and acid; 20.7wt% of deionized water.

[0115] (2) Reaction of polyester intermediate with polycarboxylic acid and polyhydric alcohol to synthesize resin with polyester polyol: add dihydric alcohol, trih...

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Abstract

The invention belongs to the chemical industry field, and relates to a preparation method of high-performance aqueous polyester polyol dispersoid. The preparation method comprises the following steps: firstly enabling dicarboxylic acid with a sulphonate-SO3M group to react with diatomic alcohol to obtain a polyester intermediate, enabling a certain amount of polyester intermediate to react with polybasic carboxylic acid and polyhydric alcohol to synthesize polyester resin with hydroxyl, and then directly adding de-ionized water to disperse so as to obtain the aqueous polyester polyol dispersoid. The aqueous polyester polyol dispersoid prepared by the invention has the characteristics of no organic solvent, high solid content, low viscosity, high storage stability, no need of neutralization by amine neutralizer and simple preparation method, and is mainly used for preparing high-performance coating material. For example, the polyester polyol dispersoid can be used with water-based polyisocyanate curing agent for preparing water-based bi-component polyurethane coating, and can also be used with water-based amine resin curing agent as water-based automobile finish.

Description

technical field [0001] The invention belongs to the field of chemical coatings, and relates to a preparation method of a high-performance polyester polyol aqueous dispersion. Background technique [0002] Since the promulgation and implementation of the first volatile organic compound (VOC) law in California, USA in 1966, the work of countries to strictly control VOC emissions and limit the production and use of high-VOC coating products has been raised to the height of laws and regulations, water-based coatings Because of its low VOC content and no need for special construction equipment, it has become one of the main directions for the development of coatings. Polyester resin coatings have attracted extensive attention due to their high gloss, high hardness, high impact resistance, good weather resistance, solvent resistance and aging resistance. Therefore, the research and development of new water-based polyester resins has become a hot spot in the development of water-ba...

Claims

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Application Information

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IPC IPC(8): C08L67/02C08L67/00C08J3/03C08G63/688C09D175/06
Inventor 刘娅莉任娜娜余喜红惠海军
Owner HUNAN UNIV
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