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Preparation method of modified carboxyl-terminated hyperbranched polyester resin and coating containing resin

A hyperbranched polyester and carboxyl-terminated technology, which is applied in the field of polyester resin, can solve problems such as cracking, poor flexibility, inconvenient and quick use, etc., and achieve high heat resistance, good flexibility, good heat resistance and flexibility Effect

Active Publication Date: 2013-03-20
HANGZHOU JIHUA POLYMER MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The coating has excellent weather resistance, good adhesion and elasticity, but the modified polyester must be used in conjunction with a polyurethane curing agent, which has the disadvantage of being inconvenient and quick to use
In the invention patent application with the publication number CN 102504293A, the modified silicone resin prepared by carboxyl-terminated hyperbranched polyester has significantly improved the mechanical properties, chemical resistance and water resistance of the silicone resin, but the flexibility is poor and high It will crack under low temperature alternating conditions, which limits its application

Method used

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  • Preparation method of modified carboxyl-terminated hyperbranched polyester resin and coating containing resin
  • Preparation method of modified carboxyl-terminated hyperbranched polyester resin and coating containing resin
  • Preparation method of modified carboxyl-terminated hyperbranched polyester resin and coating containing resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) Preparation of modified carboxyl-terminated hyperbranched polyester resin

[0037] a) Composition:

[0038] Diol: neopentyl glycol 104g (1mol);

[0039] Tribasic acid: 1,3,5-benzenetricarboxylic acid 210g (1mmol)

[0040] Silanol: Shin-Etsu KR220L 5.2g

[0041] Xylene: 2.08g

[0042]Silicone oligomer: Shin-Etsu silicone resin KR150 156g

[0043] Epoxy resin: dicyclopentadiene dioxide 10g;

[0044] Crosslinking catalyst: tetrabutyl titanate 1.04g;

[0045] Organic solvent: propylene glycol methyl ether acetate 300g;

[0046] b) synthesis steps:

[0047] Mix dibasic alcohol and tribasic acid evenly, heat to 70°C, add silanol and xylene; heat at 180°C for 1 hour, heat up to 240°C, heat for 1 hour; cool down to 90°C, add 1.0% of the weight of trihydric alcohol Double the amount of organic solvent, silicone oligomer, epoxy resin and cross-linking catalyst; heat to 110°C for 2 hours; cool down to 90°C, and finally add the remaining organic solvent.

[0048] c) Pro...

Embodiment 2

[0065] 1) Preparation of modified carboxyl-terminated hyperbranched polyester resin

[0066] a) Composition:

[0067] Diols: 62.4g (0.6mol) of neopentyl glycol; 36g (0.4mol) of 2-methyl-1,3 propanediol;

[0068] Tribasic acid: 1,2,4-benzenetricarboxylic acid 210g (1.0mol), 1,3,5-benzenetricarboxylic acid 105g (0.5mol) Silanol: Hepta(cyclopentyl)silsesquioxane trisilicon Alcohol 4.84g, Heptaisobutylsilsesquioxane Trisilanol 5.0g Xylene: 9.84g

[0069] Silicone oligomer: Shin-Etsu silicone resin KR150 100g, Shin-Etsu KR21247.6g

[0070] Epoxy resin: trimethylolpropane glycidyl ether 49.2g;

[0071] Cross-linking catalyst: tetrabutyl titanate 4.9g

[0072] Organic solvent: propylene glycol methyl ether acetate 147g butanol 23g

[0073] b) synthesis steps:

[0074] Mix dibasic alcohol and tribasic acid evenly, heat to 90°C, add silanol and xylene; heat at 200°C for 3 hours, heat up to 220°C, heat for 2 hours; cool down to 90°C, add propylene glycol methyl ether acetate, Sil...

Embodiment 3

[0090] 1) Preparation of hydroxy silicone oil

[0091] a) Formula

[0092] Octamethylcyclotetrasiloxane: 200g

[0093] Tetramethylammonium hydroxide: 0.02g

[0094] Water: 7.4g

[0095] DMF: 60g

[0096] b) Preparation process

[0097] Add octamethylcyclotetrasiloxane, tetramethylammonium hydroxide and DMF sequentially in the reactor equipped with condenser tube, thermometer, dropping funnel and stirrer, then start stirring and raise the temperature to 90°C Finally, keep the temperature constant, and add distilled water dropwise under stirring. After the dropwise addition is completed, after 9.5 hours of constant temperature reaction, the temperature is raised to 150°C for 1 hour, and the temperature is lowered to 80°C. Start vacuum distillation, and the pressure is controlled at 0.06MPa, and the reaction is evaporated. The small molecules produced in the process were cooled to room temperature, and the solid content was adjusted to 60% to obtain 157 g of hydroxyl silicon...

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Abstract

The invention relates to a preparation method of a modified carboxyl-terminated hyperbranched polyester resin. The method comprises the following steps of: mixing diol and triacid uniformly, then heating the mixture to 70-90 DEG C and adding silanol and dimethylbenzene; heating the materials at 180-210 DEG C for 1-3 hours, then continuously raising the temperature to 220-240 DEG C and carrying out heating for 1-3 hours; then reducing the temperature to 90 DEG C and adding organic solvents, organic silicon oligomers, epoxy resins and crosslinking catalysts; raising the temperature to 110-120 DEG C and carrying out heating for 2-3 hours; and finally reducing the temperature to 90 DEG C, adding other organic solvents and regulating the solid content to be 60-70%. The preparation method has the beneficial effects that as silanol is added when carboxyl-terminated hyperbranched polyester is synthesized, the heat resistance and flexibility of polyester are improved; as the organic silicon oligomers and polyester are subjected to crosslinking reaction, the heat resistance of polymer is improved; and the polyester resin prepared by the method can be used for preparing a coating with high temperature resistance and good flexibility.

Description

technical field [0001] The invention relates to the field of organic polymer compounds, and relates to a polymer compound obtained by an esterification reaction, in particular to a polyester resin. Background technique [0002] Polyester resin has excellent metal adhesion, good physical and mechanical properties such as high hardness and good chemical corrosion resistance, and is widely used in the coating industry. However, polyester resin has the disadvantages of poor heat resistance, low water resistance and poor weather resistance, which limit its application in high temperature resistant coatings. In order to improve the high temperature resistance of polyester resin, other resins are often used to chemically modify it. Silicone resin is an organic-inorganic hybrid material with excellent heat resistance, weather resistance, water resistance and low surface tension. Using silicone resin to modify polyester resin can improve the heat resistance, water resistance and ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/695C08G63/85C09D167/00
Inventor 刘海兵李希
Owner HANGZHOU JIHUA POLYMER MATERIAL CO LTD
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