Method for preparing uvioresistant polyester by nanometer titania generated in situ
A technology of in-situ generation of nano-titanium dioxide, applied in rayon manufacturing, fiber chemical characteristics, textiles and papermaking, etc., can solve problems such as agglomeration and uneven dispersion, low material strength, poor fiber spinnability and mechanical properties, etc. Achieve the effect of reducing catalytic activity and improving hue
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Embodiment 1
[0018] In a reactor with a stirrer and a distillation device, add 100 ml of ethylene glycol, and perform vigorous stirring and ice-water bath cooling; in a protective atmosphere of N 2 Then, slowly add 10ml of titanium tetrachloride, stir for 30 minutes, remove the cooling device, slowly introduce dry ammonia gas through the separatory funnel, when the solution is neutral, keep stirring for 20 minutes, let stand to cool to Normal temperature, filtered to obtain easily hydrolyzed liquid; then moved into a decompression device, distilled at a vacuum degree of 1000Pa and a temperature of 80°C, after 15 minutes, a large amount of white precipitates were formed, left to cool to normal temperature, filtered, and acetone was used. The filtrate was washed and dried to obtain a titanium glycol salt solid.
[0019] Add 1470 grams of ethylene glycol to a 2000mL beaker, add 30 grams of polyvinylpyrrolidone under stirring, heat to 70°C, and after the polyvinylpyrrolidone is completely diss...
Embodiment 2
[0024] Disperse the modified ethylene glycol salt in ethylene glycol according to the method described in Example 1, the difference is that the solid content of the slurry is 15%, and the selected organic modifier is polyethylene glycol. The amount of ethylene glycol used was 8.5 grams (6% based on the resulting nano-titanium dioxide).
[0025] 8000g of terephthalic acid, 2330g of ethylene glycol and 1960 grams of the above-mentioned titanium ethylene glycol salt / ethylene glycol slurry were beaten together and added to a 30-liter polyester polymerization kettle, and ethylene glycol antimony was used as a polycondensation catalyst, phosphoric acid three Methyl ester is a polymerization stabilizer for polymerization. Esterification is carried out under normal pressure, and the pressure in the autoclave in the final stage of polycondensation should be kept below 80Pa. After maintaining high vacuum for 185 minutes, the material is discharged to obtain nano-titanium dioxide / polyes...
Embodiment 3
[0029] Disperse the modified ethylene glycol salt in ethylene glycol according to the method described in Example 1, except that the solid content of the slurry is 22.5%, and the organic modifier is silane coupling agent KH560, KH560 The amount used is 0.56 grams (2% calculated on the basis of the nano-titanium dioxide produced).
[0030] 8000g of terephthalic acid, 3800g of ethylene glycol and 260g of the above-mentioned titanium glycol salt / ethylene glycol slurry were beaten together and added to a 30-liter polyester polymerization kettle, using ethylene glycol antimony as a polycondensation catalyst, phosphoric acid. Trimethyl ester is a polymerization stabilizer for polymerization. Esterification is carried out under normal pressure, and the pressure in the autoclave in the final stage of polycondensation should be kept below 80Pa. After maintaining high vacuum for 230 minutes, the material is discharged to obtain nano-titanium dioxide / polyester composite material. The re...
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