Preparation method of ultralow-metal ion content pyromellitic dianhydride
A technology of pyromellitic dianhydride and metal ions, applied in the field of preparation of pyromellitic dianhydride, can solve the problems of heavy vinegar smell, large corrosion of solvent equipment, large environmental protection problems, etc., and achieves the effect of broad development prospects
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Embodiment 1
[0020] A mixed gas of 1,2,4,5-tetramethylbenzene and air with a purity of 96-97% by weight, the concentration of 1,2,4,5-tetramethylbenzene in the mixed gas is 1-5 mol%, At 400°C, enter a stainless steel tubular reactor with an inner diameter of 25mm and a length of 2500mm at a speed of 4500m / min. The airflow flows from bottom to top. The tubular reactor is filled with an oxidation catalyst of 650g. The catalyst composition is vanadium pentoxide 33wt %, 63% by weight of titanium dioxide, 3% by weight of sodium oxide and 1% by weight of phosphorus pentoxide, the catalyst is carried on silicon carbide spheres, and the weight of the catalyst is 13% by weight of the carrier. The mixed gas of 1,2,4,5-tetramethylbenzene and air is catalyzed and oxidized through the catalyst layer, and then pyromellitic acid is first converted into crude pyromellitic anhydride at 425°C, and the mixed gas passes through the heat exchanger Cooling; the temperature of the cooled stream drops to 300°C, a...
Embodiment 2
[0022] In addition to the catalyst weight composition is vanadium pentoxide 32% by weight, titanium dioxide 62% by weight, sodium oxide 1% by weight, and phosphorus pentoxide 5% by weight, the oxidation reaction temperature is 426 ° C, and the temperature of the stream cooled by the heat exchanger is 250 °C °C, adsorbent molecular sieve 5A: silica is equal to 2:80 (weight ratio), the weight of silica gel G is 3% by weight of the total weight of molecular sieve 5A and silica, and the filling height of adsorbent is 300mm. When the crude pyromellitic dianhydride is collected, the temperature is 180°C, and the crude pyromellitic dianhydride is recrystallized with a mixed solvent of petroleum ether and dimethylacetamide, and the mixing weight ratio of petroleum ether and dimethylacetamide solvent is 50 : 50, corresponding to 1,2,4,5-tetramethylbenzene, except that the yield of purified pyromellitic dianhydride is 42%, other operating processes and product quality indicators are the ...
Embodiment 3
[0024] In addition to the weight of the catalyst, the composition is 30% by weight of vanadium pentoxide, 64% by weight of titanium dioxide, 5% by weight of sodium oxide and 1% by weight of phosphorus pentoxide. The oxidation reaction temperature is 380°C, and the temperature of the stream cooled by the heat exchanger is 350°C. , adsorbent molecular sieve 3A: silica is equal to 20:98 (weight ratio), the weight of silica gel G is 5% by weight of the total weight of molecular sieve 3A and silica, the adsorbent filling height is 400mm, and the The stream temperature is 220°C, and the crude pyromellitic dianhydride is recrystallized with a mixed solvent of butanone and dimethylformamide. The mixing ratio of the two solvents is 40:60, corresponding to 1,2,4,5-tetramethyl Benzene, the yield of pure pyromellitic dianhydride is 40%, other operation process, product quality index and embodiment 1 are identical.
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