Preparation method of catalytic ceramic filter tube based on 3D printing technology
A 3D printing and ceramic technology, which is applied in the direction of catalyst activation/preparation, ceramic products, chemical instruments and methods, etc., can solve the problem that the uniformity and thickness controllability of the catalyst need to be improved, which affects the permeability of the catalytic ceramic filter tube and the poor uniformity of the catalyst. and other problems, to achieve excellent fluidity, promote diffusion speed, and promote the effect of wrapping
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Embodiment 1
[0027]Preparation of Heptagonal POSS sodium salt: put 0.01mol phenyltrimethylsilane, 120mL tetrahydrofuran, 3mL deionized water and 0.036mol sodium hydroxide in a single-necked flask with magnetic stirring, stir and heat up to reflux, keep Reflux reaction, when a small amount of white solid precipitates out of the reaction system, drop to room temperature and continue to stir the reaction for 24h, spin dry the solvent, and vacuum dry to obtain heptagonal POSS sodium salt.
Embodiment 2
[0029] Preparation of bromopropyl-POSS:
[0030] Add 0.1 mol of Heptagonal POSS sodium salt prepared in Example 1 into a three-necked flask, under nitrogen protection, add 120 mL of anhydrous tetrahydrofuran, stir evenly, add 0.21 mol of triethylamine, react in an ice bath at 0°C for 1 h, and use a constant pressure funnel Slowly add 60mL of tetrahydrofuran solution containing 0.23mol 3-bromopropyltrichlorosilane dropwise, the rate of addition is 2 drops / sec, react for 6h, then rise to room temperature for 12h, filter after the reaction, spin dry the filtrate and separate it through a column ( The volume ratio of dichloromethane:petroleum ether is 1:2), and vacuum-dried to constant weight to obtain bromopropyl-POSS.
Embodiment 3
[0032] Preparation of modified polyethylene glycol:
[0033] The first step is to dissolve 200 g of polyethylene glycol in deionized water, stir and heat up to 60 ° C until the polyethylene glycol is completely dissolved, then add 20 g of oxidant, and react in an open mouth for 2 hours to obtain carboxylated polyethylene glycol, wherein the oxidant is It is composed of 68wt% nitric acid solution and 4-hydroxy-2,2,6,6-tetramethyl-piperidine nitroxide radical (nitric acid, 4-hydroxy-2,2,6,6-tetramethyl-piperidine The molar ratio of nitroxide radicals is 1:1), and the relative molecular mass of polyethylene glycol is 2000;
[0034] In the second step, 100g of carboxylated polyethylene glycol and 20g of bromopropyl-POSS prepared in Example 2 were added to 150mL of N,N-dimethylformamide. After mixing, 0.1g of potassium fluoride and 0.14mol of potassium fluoride were added. Triethylamine, heated to 95°C, stirred and reacted for 4h, cooled to room temperature, extracted twice with a...
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