Synthetic method of phosphate modified urethane acrylate

A technology of polyurethane acrylate and synthesis method, which is applied in the direction of polyurea/polyurethane adhesive, adhesive type, adhesive, etc., can solve the problems of unseen synthesis method and application, etc., and achieve high functionality and good flexibility , the effect of reducing the dosage

Inactive Publication Date: 2009-11-18
山西省应用化学研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Directly introducing phosphoric acid groups into the long chain of polyurethane acrylate can reduce its production cost, improve the solu

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 400g of polyether diol (Mn=400, 1.00mol) into a 1000ml four-neck flask, vacuum dehydrate at 90-100°C for 1 hour, cool down to 30°C, add 101g (1.00mol) of triethylamine, 50g of toluene , Slowly add 51.2g (0.33mol) POCl dropwise at this temperature 3 After the dropwise addition, react at 40° C. for 3 hours, wash the product with water until neutral, separate layers, and distill under reduced pressure to obtain 398 g of hydroxyl-terminated polymer (hydroxyl value 135.3 mgKOH / g). Add the product dropwise to 213g (0.96mol) IPDI, keep the temperature at 70°C, and add 113.2g (0.98mol) hydroxyethyl acrylate and 2 drops of dibutyltin dilaurate to the vicinity of the theoretical isocyanate value. React at 75°C until the NCO characteristic peak cannot be detected by infrared, and then the phosphate-modified polyurethane acrylate is obtained.

Embodiment 2

[0030] Add 450g of polyester diol (Mn=600, 0.75mol) into a 1000ml four-necked bottle, vacuum dehydrate at 90-100°C for 1 hour, cool down to 30°C, add 75.8g (0.75mol) of triethylamine, 50g Toluene, slowly drop 38.4g (0.25mol) POCl at this temperature 3 After the dropwise addition, react at 50° C. for 2.5 hours, wash the product with water until neutral, separate layers, and distill under reduced pressure to obtain 391 g of a hydroxyl-terminated polymer (hydroxyl value: 91.3 mgKOH / g). Add this product dropwise to 111.4g (0.64mol) 80 / 20TDI, keep the temperature at 70°C, and add 75.1g (0.65mol) of hydroxyethyl acrylate and 2 drops of dibutyltin dilaurate to near the theoretical isocyanate value The catalyst is reacted at 75°C until the NCO characteristic peak is not detected by infrared, and the product is obtained.

Embodiment 3

[0032]Add 500g of polyether diol (Mn=1000, 0.5mol) into a 1000ml four-necked bottle, vacuum dehydrate at 90-100°C for 1 hour, cool down to 30°C, add 50.5g (0.5mol) of triethylamine, 50g Toluene, slowly drop 26.1g (0.17mol) POCl at this temperature 3 In a four-neck flask, react at 35° C. for 4 hours after the dropwise addition, wash the product with water until neutral, separate layers, and distill under reduced pressure to obtain 475 g of a hydroxyl-terminated polymer (hydroxyl value 55 mgKOH / g). Take 200g of this product and add dropwise to 33.6g (0.2mol) HDI, keep the temperature at 60°C, and add 27.3g (0.21mol) of hydroxyethyl methacrylate and 1 drop of dilauric acid dilaurate to the vicinity of the theoretical isocyanate value. Butyl tin catalyst, react at 70°C until the NCO characteristic peak is not detected by infrared, and the product is obtained.

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Abstract

A synthetic method of phosphate modified urethane acrylate comprises the steps of adopting POCl3 and long chain diol to synthesize hydroxyl terminated polymer, using the hydroxyl terminated polymer and excessive diisocyanate to synthesize an isocyanato terminated polymer, and finally grafting the isocyanato terminated polymer by hydroxyl acrylate to generate the phosphate modified urethane acrylate. As the phosphate modified urethane acrylate synthesized by the method in the invention has big functionality and low viscosity, the phosphate modified urethane acrylate can be used in ultraviolet-cured adhesives and is capable of reducing dosage of a reactive diluent and improving the mechanical properties of cured film. The light-cured glue film has excellent flexibility, adhesion force and bonding strength, and can be widely applied to glass and metal base materials for improving the mechanical properties thereof such as the adhesion force and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer compound synthesis, and relates to a method for synthesizing ultraviolet-curable polyurethane acrylate, in particular to a method for synthesizing phosphate-modified polyurethane acrylate. The phosphate-modified urethane acrylate of the invention is especially suitable for metal and glass substrates to improve the adhesion of ultraviolet light curing systems. Background technique [0002] Due to the advantages of fast curing speed, no solvent volatilization, and energy saving, UV curing system has gradually been widely used in adhesives, coatings, inks and other fields in the late 20th century. In recent years, with the development of light curing technology, light curing materials have been widely used in chemical industry, machinery, light industry, communication and other fields, not only in wood, metal, plastic, paper, leather, but also in optical fiber, printing It has been successfully appl...

Claims

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Application Information

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IPC IPC(8): C08G18/83C08G18/64C09J175/14
Inventor 马国章吴建兵侯彩英牛润林马小龙蒋迎忠
Owner 山西省应用化学研究所
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