Preparation method of melamine ring-containing triphosphonate doped PBI high-temperature proton exchange membrane

A technology of proton exchange membrane and triphosphonate, which is applied in the direction of final product manufacturing, sustainable manufacturing/processing, electrochemical generator, etc., can solve the problems of reducing the proton conductivity of composite membranes and the relative content of proton conductors, and achieve The effects of environmental friendliness, high yield, and simple preparation method

Active Publication Date: 2020-05-29
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of cross-linking agent is related to its cross-linking degree. The mechanical properties, size and chemical stability of PBI membrane usually increase with the increase of

Method used

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  • Preparation method of melamine ring-containing triphosphonate doped PBI high-temperature proton exchange membrane
  • Preparation method of melamine ring-containing triphosphonate doped PBI high-temperature proton exchange membrane
  • Preparation method of melamine ring-containing triphosphonate doped PBI high-temperature proton exchange membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] [Example 1]: the preparation of TTDP:

[0032] Take 60mL of dry treated triethyl phosphite (TEP, 0.34mol) into a 200mL three-neck round bottom flask. Under magnetic stirring, 11.1g of cyanuric chloride (TCT, 0.06mol) was divided into three batches, and slowly added to triethyl phosphite within 1 hour at room temperature, TCT gradually dissolved, and the reaction released a large amount of heat, and released ethyl chloride alkane gas to obtain a yellow transparent solution. After adding TCT, raise the temperature to 100-105°C for 8 hours, cool to 50°C, slowly add 35mL of petroleum ether (boiling range 60-90°C), continue to stir and cool to room temperature, and stir overnight, a large amount of colorless crystals are precipitated. Suction filtration, wash 3 times with 20mL petroleum ether, remove unreacted TEP and TCT, obtain colorless crystal 22.9g, namely 1,3,5-triazine-2,4,6-triphosphate ethyl ester (TTDP, produced rate: 78%).

[0033] Adopt same reaction step, the...

Embodiment 2

[0036] [Example 2]: the preparation of TPT:

[0037] Add 19.6g TTDP (0.04mol) into 130mL concentrated hydrochloric acid, reflux for 36h under magnetic stirring, cool to 50°C, distill off HCl under reduced pressure, concentrate to 40mL, extract three times with 90mL ethyl acetate to remove unhydrolyzed TTDP. The aqueous phase was concentrated to nearly dryness, and dried in a vacuum oven at 120° C. for 12 hours to obtain 12.3 g of a white solid, namely 1,3,5-triazine-2,4,6-triphosphoric acid (TPT, yield: 96% ).

[0038] Using the same reaction steps, but extracting with dichloromethane, benzene, toluene or petroleum ether, the yields were 94%, 89%, 91% and 85%, respectively.

[0039] Using the same reaction steps, reflux in concentrated hydrochloric acid for 12h, distill under reduced pressure at 70°C, and extract with ethyl acetate, the yield is 84%.

[0040] The hydrolysis of different ester groups of TTDP prepares the productive rate of TPT as shown in Table 2:

[0041] T...

Embodiment 3

[0043] [Example 3]: Preparation of CeTPT-1:2

[0044] Take 9.63g TPT (0.03mol) and add it into 20mL deionized water, stir at room temperature for 30min to fully dissolve it. Take 8.76g dihydrate cerium ammonium nitrate (0.015mol) and dissolve it in 30mL0.1mol L- 1 In dilute hydrochloric acid (to avoid hydrolysis to generate insoluble cerium hydroxide). Add the hydrochloric acid solution of ammonium cerium nitrate dropwise to the aqueous solution of TPT, and stir at room temperature for 12 hours to make the phosphonic acid group on TPT and Ce 4+ The polymerization reaction was fully carried out in between, and a yellow suspension was obtained. Suction filtration, washing with deionized water until the filtrate pH = 7, to fully remove unreacted raw materials, dried at 120 ° C for 12 hours, to obtain 6.0 g of yellow solid (yield 51%), wherein the molar ratio of cerium and TPT is 1 :2, that is, cerium 1,3,5-triazine-2,4,6-triphosphate (CeTPT-1:2).

[0045] The preparation of t...

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Abstract

The invention discloses a preparation method for preparing a proton exchange membrane, used at a high temperature and a low humidity, by doping polybenzimidazole (PBI) (PBI can contain a pyridyl group, a pyrazinyl group or an imidazolyl group) with melamine ring-containing triphosphonate (MTPT, wherein the metal ion M is Zr<4+>, Ce<4+>, Fe<3+>, La<3+> or Y<3+> ) serving as a proton conductor. Thepreparation method comprises the following steps: firstly, preparing the insoluble melamine ring-containing triphosphonate (MTPT) through a three-step reaction, doping the novel PBI with the MTPT, andcrosslinking to form the composite high-temperature and low-humidity proton exchange membrane. The composite membrane is used in the fields of hydrogen-oxygen fuel cells, direct methanol fuel cells or methanol reformed fuel cells, operated at high temperature and low humidity, high-temperature electrolysis, sensors and the like.

Description

technical field [0001] The invention relates to a preparation method of a proton exchange membrane in a high-temperature and low-humidity fuel cell, which can be used in the fields of solid acid catalysts, catalytic membrane separation reaction devices, fuel cell proton exchange membranes, electrolytic membranes, permeable membranes, sensor materials and the like. [0002] technical background [0003] As a kind of fuel cell, proton exchange membrane fuel cell has attracted widespread attention because of its environmental protection, pollution-free, high energy conversion rate, high power density and low operating temperature. Proton exchange membrane is the core component of proton exchange membrane fuel cell, its quality directly affects the performance and service life of proton exchange membrane fuel cell, so the research on proton exchange membrane is particularly important. In order to ensure that the proton exchange membrane fuel cell has good performance, it is neces...

Claims

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Application Information

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IPC IPC(8): C08L79/04C08K5/00C08J5/22H01M8/1072
CPCC08J5/2256C08K5/0091H01M8/1072C08J2379/04Y02P70/50
Inventor 孙鹏李忠芳郭辉王燕崔伟慧
Owner SHANDONG UNIV OF TECH
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