A kind of preparation method of speek/mcm composite diaphragm
A composite diaphragm, vanadium oxidation technology, applied in fuel cells, regenerative fuel cells, electrical components, etc., can solve the problems of high cost and vanadium ion penetration price, achieve low internal resistance, improve mechanical properties and chemical stability, and reduce costs. Effect
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Embodiment 1
[0043] In this example, the preparation method of the sulfonated polyether ether ketone / modified carbonaceous mudstone composite diaphragm is as follows:
[0044] 1. Preparation of MCM: Dissolve carbonaceous mudstone solids in sulfuric acid with a molar concentration of 1M to a mass-volume ratio of 1 / 5 (g / mL). The reaction was stirred at room temperature and 1500r / min for 2h. After the reaction, the precipitate was centrifuged and washed with deionized water until neutral, and dried in an oven for 24h to obtain a dry solid. The dried solid was heated under reflux and stirred for 12 hours with nitric acid with a molar concentration of 3M. After the reaction, the precipitate was centrifuged and washed with deionized water to neutrality, and dried in an oven for 24 hours to obtain dry functionalized carbonaceous mudstone MCM powder. . Such as figure 1 As shown, the obtained dry functionalized modified carbonaceous mudstone MCM powder has a particle size of 200-700nm.
[0045] ...
Embodiment 2
[0057] The difference from Example 1 is:
[0058] 150 mg of MCM powder was weighed and added into the SPEEK solution, and the rest of the steps in Example 1 were used to prepare the SPEEK / MCM composite diaphragm. Wherein, the MCM content of the SPEEK / MCM mixed solution is 5wt%.
[0059] In this example, the thickness of the obtained SPEEK / MCM composite diaphragm is 68 μm, the texture of the composite diaphragm is uniform and dense, there is no MCM dissolution phenomenon, and it has good flexibility and mechanical properties.
[0060] The relevant performance data of the present embodiment are as follows:
[0061] The battery test using the separator at room temperature shows that the composite separator vanadium battery prepared at this ratio has good performance, but the capacity retention is worse than that of the separator prepared in Example 1, which is not conducive to the long-term cycle of the vanadium battery. Compared with the preparation of the separator in Example...
Embodiment 3
[0063] The difference from Example 1 is:
[0064] Weigh 600 mg of MCM powder and add it into the SPEEK solution, and use the rest of the steps in Example 1 to prepare the SPEEK / MCM composite diaphragm. Wherein, the MCM content of the SPEEK / MCM mixed solution is 20wt%.
[0065] In this example, the thickness of the obtained SPEEK / MCM composite diaphragm is 72 μm, and the texture of the composite diaphragm is uniform, but the MCM has agglomeration and dissolution phenomenon, which is not suitable for application in vanadium batteries.
[0066] The results of the examples show that the present invention uses a dissolution method to prepare a SPEEK solution, uses the functionalized MCM as a proton selective conduction channel, and adopts film-forming methods such as step-by-step dispersion and solution casting to prepare a SPEEK / MCM composite diaphragm. The composite membrane prepared by the invention has the advantages of good proton selective conductivity, excellent vanadium io...
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Abstract
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