Polyether polyol for flame-retardant polyurethane rigid foam and preparation method thereof
A technology of polyether polyol and polyurethane rigid foam is applied in the field of polyether polyol for flame retardant polyurethane rigid foam and its preparation, which can solve the problems of influence of polyether polyol performance, low flame retardant efficiency and high cost, and achieves Overcome inherent defects, excellent flame retardant effect, and solve the effect of poor durability
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Embodiment 1
[0027] This embodiment provides a preparation method of polyether polyol for flammable polyurethane rigid foam:
[0028] (1) Crude flame-retardant polyether polyol: Add 133g polyphosphoric acid and 270g (1:2) pentaerythritol into a 3L autoclave under the conditions of 60°C and 1MPa, and react under reflux for 3h to obtain the first mixture; Then add 75g (3.6) glycerol and 10g potassium hydroxide to the first mixture, stir and raise the temperature to form a second mixture, blow in nitrogen for 3 times, vacuum to remove water; then raise the temperature to 90°C and control the reaction pressure to 0.1 MPa, 540g (2:1) of ethylene oxide is added to the second mixture by continuous feeding, then the temperature is raised to 110°C, the temperature is kept for 2h, and the reaction pressure is controlled to 0.05-0.1MPa for reaction to obtain crude flame retardant Polyether polyol;
[0029] (2) Refined flame-retardant polyether polyol: After adding 1.5% of its own mass of phosphoric acid ...
Embodiment 2
[0031] This embodiment provides a preparation method of polyether polyol for flammable polyurethane rigid foam:
[0032] (1) Crude flame-retardant polyether polyol: Add 135g of polyphosphoric acid and 337g of pentaerythritol to a 3L autoclave at 70°C and 1MPa, and react under reflux for 3h to obtain the first mixture; Add 85g of sorbitol, 10g of potassium hydroxide, stir and raise the temperature to form a second mixture, blow in nitrogen for 3 times, vacuum to remove water; then raise the temperature to 100°C, control the reaction pressure to 0.1MPa, and use continuous Adding 1011g of propylene oxide in the way of feeding, then heating to 110°C, holding for 2h, controlling the reaction pressure to 0.05-0.1MPa for reaction, and obtaining crude flame-retardant polyether polyol;
[0033] (2) Refined flame-retardant polyether polyol: After adding 1.5% of its own mass of phosphoric acid and 0.8% of adsorbent to the crude flame-retardant polyether polyol, it is filtered and dried.
experiment example 1
[0047] Take equal amounts of the polyether polyols provided in Examples 1-2 and Comparative Examples 1-3 and set them as experimental groups 1-5, and perform performance characterization and application characterization of experimental groups 1-5 as follows:
[0048] 1.1 Performance characterization
[0049] (1) Determination of hydroxyl value: Weigh 2.0 g (accurate to 0.0001 g) of a sample into an iodine flask, add 15 mL of acetylation reagent to it, and mix well to dissolve the sample completely. React in a water bath at 60°C for 30 minutes, take it out, and cool to room temperature, then add 20 mL of pyridine solution, 2 drops of phenolphthalein indicator, and titrate with NaOH standard solution until the solution turns pink. The end of the titration is that the color does not fade within 15 seconds. At the same time, a blank test is performed, and the hydroxyl value calculation formula is as follows:
[0050] Hydroxyl value / mgKOH.g -1 =(V 1 -V 2 )c×56.1 / m
[0051] Where: V 1 -The...
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Abstract
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