Toluene diisocyanate trimer preparation method
A technology of toluene diisocyanate and toluene diisocyanate containing toluene diisocyanate is applied in the field of preparing toluene diisocyanate trimer, can solve the problems of strong corrosiveness of phenolic compounds, high production condition requirements, increase production cost and the like, and achieves narrow molecular mass distribution, The effect of improving quality and yield, and easy separation
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Embodiment 1
[0018] Weigh 10g of sodium montmorillonite whose particle size is controlled to be less than 60 microns and 210g of distilled water to make a suspension, and 5g of cetyltrimethylammonium bromide to make a 10% aqueous solution with a mass fraction of distilled water. Add the aqueous solution of cetyltrimethylammonium bromide to the suspension of montmorillonite and stir at 70°C for 3 hours, filter and wash with distilled water repeatedly until the filtrate is washed with 0.1mol / L AgNO 3 Test without Br - . The obtained organic montmorillonite was vacuum-dried in a vacuum oven at 60° C. for 24 hours, ground by a ball mill, and sieved to control the particle size to be less than 60 microns.
[0019] Add 25g of toluene diisocyanate into a three-necked flask containing 75g of anhydrous butyl acetate, stir at 50°C for 15min, and measure the -NCO content by sampling with di-n-butylamine titration. Add 1g of organic montmorillonite, stir, control the temperature at about 50°C, react...
Embodiment 2
[0021] The preparation method of organomontmorillonite is the same as in Example 1.
[0022] Add 5 g of toluene diisocyanate into a three-neck flask containing 95 g of toluene, stir at 20°C for about 1 min, and measure its -NCO content by di-n-butylamine titration. Add 0.5g of organic montmorillonite, stir, control the temperature at about 30°C, react for 8 hours to terminate the reaction, centrifuge and take the supernatant to obtain the product. -1 、1420cm -1 、760cm -1 There is a characteristic absorption peak of isocyanurate, 13 The peak of C-NMR spectrum δ148.6-δ149.1 belongs to the carbonyl peak in trimeric isocyanurate, indicating that the product is toluene diisocyanate trimer. Product yield 7.2%.
Embodiment 3
[0024] Organomontmorillonite with the brand name HFGEL-140 was purchased from Zhejiang Fenghong Clay Chemical Co., Ltd.
[0025] Add 50g of toluene diisocyanate into a three-necked flask containing 50g of anhydrous butyl acetate, stir at 100°C for about 60min, and measure its -NCO content by di-n-butylamine titration. Add 10 g of organic montmorillonite, stir, control the temperature at about 100° C., react for 1 hour to terminate the reaction, and centrifuge to obtain the supernatant to obtain the product. at 1709cm -1 、1420cm -1 、760cm -1 There is a characteristic absorption peak of isocyanurate, 13 The peak of C-NMR spectrum δ148.6-δ149.1 belongs to the carbonyl peak in trimeric isocyanurate, indicating that the product is toluene diisocyanate trimer. Product yield 39%.
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