Tetra-functionality urethane acrylate based on pentaerythritol and preparation method and application tetra-functionality urethane acrylate
A technology of polyurethane acrylate and isocyanate ethyl acrylate, which is applied in the field of materials, can solve the problems of difficult control of the production process, many steps in the reaction process, and tediousness, and achieve the effects of easy control, reduced reaction steps, and low viscosity
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Embodiment 1
[0036] Drop into 1361 grams of pentaerythritol (CAS No. 115-77-5, chemical formula C in 6L autoclave 5 h 12 o 4 , molecular weight 136.15), 30 grams of sodium formate, warming up to 155 ° C, began to drop ethylene oxide (C 2 h 4 O, molecular weight 44) 2200 grams of reaction, temperature control 155 ° C ~ 165 ° C, pressure 0.10 ~ 0.40 MPa, dropwise for 3 ~ 4 hours, after the drop is completed, 155 ° C ~ 165 ° C for 2 ~ 3 hours, and then cooled to 80 ° C Below, the crude product is obtained in discharging; after the crude product was added 40 grams of activated clay and stirred for 30 minutes, it was clear and transparent tetrahydroxypolyether (C 15 h32 o 9 , molecular weight 356) 3488.8 grams, structure as shown in formula (I), wherein: n=2, a+b+c+d=5.
[0037] In the 1000mL four-necked flask, drop into the prepared tetrahydroxypolyether (C 15 h 32 o 9 , molecular weight 356) 178 grams, isocyanate ethyl acrylate 282.24 grams (2mol), catalyst dibutyltin dilaurate 0.3 gr...
Embodiment 2
[0042] Drop into 1361 grams of pentaerythritol (CAS No. 115-77-5, chemical formula C in 6L autoclave 5 h 12 o 4 , molecular weight 136.15), 50 grams of potassium formate, warming up to 155 ° C, began to drop propylene oxide (C 3 h 6 O, molecular weight 58) 3480 grams of reaction, temperature control 155 ° C ~ 165 ° C, pressure 0.10 ~ 0.40 MPa, dropwise for 3 ~ 4 hours, after the drop is completed, 155 ° C ~ 165 ° C for 2 ~ 3 hours, and then cooled to 80 ° C Below, the crude product is obtained in discharging; after the crude product was added 60 grams of activated clay and stirred for 30 minutes, it was clear and transparent tetrahydroxypolyether (C 23 h 48 o 10 , molecular weight 484) 4743.2 grams, structure as shown in formula (I), wherein: n=3, a+b+c+d=6.
[0043] In the 1000mL four-necked flask, drop into the prepared tetrahydroxypolyether (C 23 h 48 o 10 , molecular weight 484) 242 grams, isocyanate ethyl acrylate 280 grams (1.984mol), catalyst dibutyltin dilaura...
Embodiment 3
[0048] With reference to the method of Example 1-2 in Chinese patent ZL201310143167.9, 4-functionality polyurethane acrylate was obtained, respectively as Comparative Example 1-2, and the 4-functionality urethane acrylate obtained in Example 1-2 of the present invention and Comparative Example 1-2 was investigated. Viscosity of functional urethane acrylates.
[0049] Test method: NDJ-1 rotary viscometer, No. 4 rotor, 60 rpm. Refer to "NDJ-1 Rotational Viscometer Instruction Manual" for specific operation steps.
[0050] Table 1 Viscosity of 4-functionality polyurethane acrylate
[0051]
Comparative example 1
Example 1
Comparative example 2
Example 2
viscosity
12000mPa.s@60℃
6000mPa.s@60℃
15000mPa.s@60℃
7400mPa.s@60℃
[0052] Compared with the product of Comparative Example 1, the viscosity of the product of Example 1 decreased by 6000mPa.s@60°C, and the rate of decrease was 50.00%.
[0053] Compared with the product of ...
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