Active group closed diisocyanate for 3D object printing, composition and 3D object printing method and device
A technology of diisocyanate and active groups, which is applied in the field of 3D object printing, can solve problems that hinder the development of photocuring 3D printing technology, achieve the effects of improving dimensional stability, improving mechanical properties, and reducing manufacturing costs
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Embodiment 1
[0092] The preparation method of the 4-acrylic acid phenol-blocked diisocyanate provided in this embodiment comprises the following steps:
[0093]Step 1, under the protection of inert gas nitrogen, add hydroquinone (20.0g, 181.6mmol) and the first catalyst triethylamine (12.3g, 121.5mmol) in the dry first reaction vessel, use the first solvent Tetrahydrofuran (200ml) was dissolved, and acryloyl chloride (13.7g, 151.3mmol) was added dropwise at 0°C, the time was controlled within 30min, after the addition was completed, it was reacted at 0°C for 4h, the reaction product was filtered, and the filtrate was collected and evaporated to obtain the first product; the first product was purified by silica gel column chromatography, and dried in a vacuum oven at a temperature of 30-50°C to constant weight to obtain 4-acrylic acid phenol, the reaction formula of which is as follows:
[0094]
[0095] Step 2. Infuse a sufficient amount of nitrogen into the three-necked flask of the se...
Embodiment 2
[0100] The preparation method of the 3-acrylic acid phenol-blocked polyisocyanate provided in this embodiment comprises the steps:
[0101] Step 1, under the protection of inert gas nitrogen, add resorcinol (20.0g, 181.6mmol) and the first catalyst triethylamine (18.3g, 181.6mmol) in the dry first reaction vessel, use the first solvent Diethyl ether (200-240ml) was dissolved, and methacryloyl chloride (19g, 181.6mmol) was continuously added dropwise at 0-3°C, and the time was controlled within 30min. After the addition was completed, it was reacted at 3°C for 5h, and the reaction product was Filtrate, collect the filtrate and evaporate to obtain the first product, use silica gel column chromatography to purify the first product, and dry it in a vacuum oven at a temperature of 30-50°C to constant weight to obtain 3-methacrylic acid phenol, Its reaction formula is as follows:
[0102]
[0103] Step 2. Infuse a sufficient amount of nitrogen into the three-necked flask of th...
Embodiment 3
[0107] The preparation method of 4-acrylic acid phenol and 4-methacrylic acid phenol blocked polyisocyanate provided in this embodiment comprises the steps:
[0108] Step 1, with step 1 of embodiment 1, prepare 4-acrylic acid phenol;
[0109] Step 2, using the same method as step 1, using methacryloyl chloride as a substrate to prepare 4-methacrylic acid phenol;
[0110] Step 3, in the second reaction vessel three-necked flask, pass into enough nitrogen, get rid of air, the 4-acrylic acid phenol (5.5g, 33.4mmol) that step 1-2 prepares and 4-methacrylic acid phenol (6g , 33.4mmol) into a three-necked flask, add 12ml-20mlDMF to dissolve, then add naphthalene diisocyanate (6.4g, 30.4mmol), react at 50-60°C for 45min, then add the second catalyst Sn(Oct) 2 (0.02g), raise the temperature to 80-90°C, and react for 3-4h;
[0111] The reaction product is repeatedly washed with acetone solution, and dried to constant weight in a vacuum oven to obtain 4-acrylic acid phenol and 4-metha...
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