A kind of preparation method of polysiloxane type hydrogen-absorbing polymer film material
A polymer film, polysiloxane-type technology, applied in the directions of alkali metal oxides/hydroxides, alkali metal compounds, chemical instruments and methods, etc., can solve application difficulties, difficult hydrogen absorption properties and mechanical properties absorption. Hydrogen polymer, difficult and high hydrogen absorption materials, etc., to achieve the effect of convenient use
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Embodiment 1
[0024] (1) Preparation of Alkoxycyclotetrasiloxane
[0025]
[0026] where R is Si(OEt) 3
[0027] Weigh 20 g of tetramethylcyclotetrasiloxane and 10 ml of xylene into a 150 ml round bottom flask, and bubble nitrogen gas for 15 min to remove the air in the system. After that, 10 g of triethoxysilane and 0.1 ml of Cassette catalyst were added, and the reaction was carried out at room temperature for 24 h. After the reaction, activated carbon was added and stirred for 2 h, then filtered, and the xylene was removed under reduced pressure to obtain a slightly yellow transparent liquid.
[0028] (2) Synthesis of alkoxy grafted polyvinylmethylsiloxane
[0029]
[0030] Measure 100mL of tetramethyltetravinylcyclotetrasiloxane, 2ml of alkoxycyclotetrasiloxane and 0.2mL of hexamethyldisiloxane, add them to a 250ml single-necked flask equipped with mechanical stirring, and then add 0.1 g potassium hydroxide was used as a catalyst, and the reactant was heated to 100°C for 3h. ...
Embodiment 2
[0038] (1) Synthesis of silanol-terminated polyvinylmethylsiloxane
[0039]
[0040] Measure 100 mL of tetramethyltetravinylcyclotetrasiloxane into a single-necked flask equipped with mechanical stirring, and then add 0.1 g of potassium hydroxide. The reactant was heated to 100°C for 3h. Then add 100mL of n-hexane to dissolve the reaction product. The resulting solution is washed with dilute hydrochloric acid and then washed three times with deionized water. After layering, the organic phase is dried with magnesium sulfate, and the solvent and low molecular volatiles are removed in vacuo to obtain a colorless transparent oily liquid .
[0041] (2) Preparation of composite hydrogen-absorbing polymer
[0042] Weigh 2.0g of silanol-terminated polyvinylmethylsiloxane, add 5ml of n-hexane to dissolve, then add 0.8g of Pd / C (5wt%) and 0.03g of tetraethyl silicate, mechanically stir evenly, and then add 15μL of diethylsilicate Dibutyltin laurate, stir to mix well. The resultin...
Embodiment 3
[0048] The composite hydrogen-absorbing material obtained by mixing the prepolymers prepared in Example 1 and Example 2 at 1:1;
[0049] Weigh 1.0g of alkoxy-grafted polyvinylmethylsiloxane and 1.0g of silanol-terminated polyvinylmethylsiloxane, add 5ml of n-hexane to dissolve, and then add 0.8g of Pd / C (5wt%) , after mechanical stirring, add 15 μL of dibutyltin dilaurate, and stir to mix evenly. The resulting black mixture was poured on a glass plate, and then cured at room temperature for 2 days to obtain a black elastic composite film.
[0050] Gained black film (2.2g) is placed in the airtight container (1L) that is filled with 146KPa pure hydrogen and is tested at room temperature, and the pressure change situation of different time system is as follows:
[0051] time (hours) 2 6 10 16 24 48 96 Pressure (KPa) 105 93 88 76 71 67 63
[0052]Gained black film (0.2g) is placed in mixed gas (250mL 1% hydrogen-nitrogen mixed gas) and the hydrog...
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