Method for preparing uvioresistant polyester by nanometer titania generated in situ
A technology of nano-titanium dioxide and nano-titanium oxide, which is 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 equipped with a stirrer and a distillation device, add 100ml of ethylene glycol, and carry out vigorous stirring and ice-water bath cooling; in a protective atmosphere N 2 Slowly add 10ml of titanium tetrachloride, stir for 30 minutes, remove the cooling device, and slowly pass in dry ammonia gas through the separatory funnel. When the solution is neutral, keep stirring for 20 minutes, and let it cool down to At room temperature, filter to obtain a liquid that is easily hydrolyzed; then move it into a decompression device, distill at a vacuum of 1000 Pa and a temperature of 80 ° C, after 15 minutes, a large amount of white precipitate is formed, stand to cool to room temperature, filter, and use acetone Wash the filtrate and dry to obtain the titanium glycolate solid.
[0019] Add 1470 grams of ethylene glycol into a 2000mL beaker, add 30 grams of polyvinylpyrrolidone while stirring, and heat to 70°C. After stirring and reacting for 1 hour, set aside.
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Embodiment 2
[0024] The modified ethylene glycolate is dispersed 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, poly The consumption of ethylene glycol is 8.5 grams (6% by generating nano titanium oxide meter).
[0025] 8000g of terephthalic acid, 2330g of ethylene glycol and 1960 grams of the above-mentioned ethylene glycol salt / ethylene glycol slurry of titanium are beaten together and then added to a 30-liter polyester polymerization kettle. Antimony ethylene glycol is used as a polycondensation catalyst and phosphoric acid tris Methyl ester is a polymerization stabilizer for polymerization. Esterification is carried out under normal pressure, and the pressure in the kettle in the final stage of polycondensation should be kept below 80Pa. After maintaining a high vacuum for 185 minutes, the material was discharged to obtain a nano-titanium oxide / p...
Embodiment 3
[0029] The modified ethylene glycolate is dispersed in ethylene glycol according to the method described in Example 1, the difference is that the solid content of the slurry is 22.5%, and the organic modifier is silane coupling agent KH560, KH560 The dosage is 0.56 grams (2% based on the calculation of generating nano-titanium oxide).
[0030] 8000g of terephthalic acid, 3800g of ethylene glycol and 260g of the above-mentioned ethylene glycol salt / ethylene glycol slurry of titanium are beaten together and then 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 reaction. Esterification is carried out under normal pressure, and the pressure in the kettle in the final stage of polycondensation should be kept below 80Pa. After maintaining a high vacuum for 230 minutes, the material was discharged to obtain a nano-titanium oxide / polyest...
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