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Diaphragm for electrochemical synthesis of dinitrogen pentoxide and preparation method thereof

A dinitrogen pentoxide and electrochemical technology, applied in the direction of organic diaphragms, etc., can solve problems such as constraints, current efficiency and theoretical value gap, and achieve the effects of reducing losses, reducing diaphragm resistance, and mild conditions

Active Publication Date: 2011-12-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] It can be seen from the above that currently in the electrochemical synthesis of N 2 o 5 Among the diaphragms used in the process, the industrial application prospect of porous polytetrafluoroethylene (PTFE) membrane-inorganic hybrid membrane formed by doping with inorganic substances is good, but the existing patents and literatures are about applying to electrochemical synthetic N 2 o 5 The current efficiency of the porous polytetrafluoroethylene (PTFE) membrane-inorganic hybrid membrane in the process is still far from the theoretical value, which seriously restricts the electrochemical synthesis of N 2 o 5 technology industrialization process

Method used

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  • Diaphragm for electrochemical synthesis of dinitrogen pentoxide and preparation method thereof
  • Diaphragm for electrochemical synthesis of dinitrogen pentoxide and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 1. The porous polytetrafluoroethylene membrane adopts the purchased BS01 hydrophobic porous polytetrafluoroethylene membrane. The size of the membrane is 5cm×5cm, the pore diameter is 0.1μm, the porosity is 55%, and the thickness is 0.06mm. The base film was refluxed in acetone at a temperature of 60°C for 3 hours, then immersed in 98% nitric acid for 24 hours, rinsed with deionized water after taking it out until the pH value of the eluate was 7, and dried in vacuum at a temperature of 80°C 24h. The dry film mass was determined to be 0.5397 g by weighing.

[0025] 2. Immerse the treated BS01 hydrophobic porous polytetrafluoroethylene membrane in a 5wt% high fluorinated ion exchange resin (Nafion) solution for 24h, dry it in a vacuum oven at 80°C for 20h, and weigh it to determine that the dry film quality is 0.5580 g, swell with deionized water for 24h, and then use 0.5mol / L H 2 SO 4 The solution was swollen for 4 hours to obtain a porous polytetrafluoroethylene-hig...

Embodiment 2

[0030] Steps 1, 2, and 3 are the same as in Example 1: a highly fluorinated ion-exchange resin (Nafion) with a loading capacity of 3.3%, SiO 2 Porous polytetrafluoroethylene-highly fluorinated ion exchange resin (Nafion)-SiO with a loading of 2.2% 2 membrane;

[0031] Step 4 is different from Example 1: the expanded polytetrafluoroethylene membrane is changed to ePTFE-2 type, with a pore size of 90-100 nm, a thickness of 10-20 μm, a porosity of 90-98%, and a mechanical pressing pressure of 10 MPa. The time is 50h, and the prepared membrane is porous polytetrafluoroethylene-high fluorinated ion exchange resin (Nafion)-SiO 2 - expanded polytetrafluoroethylene (ePTFE) diaphragm;

[0032] Step 5 is different from Example 1: the anode initial solution is N 2 o 4 Concentration of 28.1% N 2 o 4 / HNO 3 , the operating voltage is 5.5V.

[0033] The experimental results are shown in Table 1.

Embodiment 3

[0035] Steps 1 and 2 are the same as in Example 1: a porous polytetrafluoroethylene-highly fluorinated ion exchange resin (Nafion) membrane with a loading capacity of 3.5% was prepared;

[0036] The difference between step 3 and embodiment 1: change the film made of above SiO 2 Soak in the sol for 12 hours, dry at room temperature, then vacuum dry in an oven at 60°C for 12 hours, weigh to determine the quality of the dry film, and obtain SiO 2 Porous polytetrafluoroethylene-highly fluorinated ion exchange resin (Nafion)-SiO with a loading of 1.0% 2 membrane;

[0037] Step 4 is the same as Example 1: the membrane obtained is porous polytetrafluoroethylene-high fluorinated ion exchange resin (Nafion)-SiO 2 - expanded polytetrafluoroethylene (ePTFE) diaphragm;

[0038] Step 5 is different from Example 1: the anode initial liquid is N 2 o 4 Concentration of 30.1% N 2 o 4 / HNO 3 , operating voltage is 4.5V.

[0039] The experimental results are shown in Table 1.

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Abstract

The invention discloses a diaphragm for electrochemical synthesis of dinitrogen pentoxide and a preparation method thereof. The diaphragm is compounded by a membrane formed by a porous polytetrafluoroethylene substrate membrane, a loaded highly-fluorinated ion exchange resin and SiO2, and an expanded polytetrafluoroethylene membrane, and has a thickness of 80-120 microns. The preparation process comprises the following steps: treating the porous polytetrafluoroethylene substrate membrane in concentrated nitric acid; loading the treated substrate membrane in a highly-fluorinated ion exchange resin solution, loading the substrate membrane loaded with highly-fluorinated ion exchange resin in SiO2 sol to obtain a porous polytetrafluoroethylene-highly-fluorinated ion exchange resin-SiO2 membrane, and pressing the membrane with an expanded polytetrafluoroethylene membrane to obtain a diaphragm for the electrochemical synthesis of dinitrogen pentoxide. The advantages of the invention are that: the diaphragm has the characteristics of low membrane resistance, high water-blocking performance, and high current efficiency; the preparation condition is mild; the production cost is low; and the preparation method facilitates industrialization.

Description

technical field [0001] The invention relates to a diaphragm for electrochemically synthesizing dinitrogen pentoxide and a preparation method thereof. The invention belongs to the technical field of dinitrogen pentoxide preparation. Background technique [0002] Electrochemically synthesized N 2 o 5 In the process, the diaphragm mainly plays the role of selectively permeating specific ions and molecules, and its performance directly affects the performance indicators such as the current efficiency and specific energy of the electrolysis. In the electrochemical synthesis of N 2 o 5 In the process, Zawadski et al. (Roznicki chemii, 1948, 22: 233-247) used porous ceramics as a diaphragm to carry out N 2 o 5 In the electrolysis process, although the current efficiency can reach 35%, the specific energy is as high as 5kWh / Kg N 2 o 5 , not suitable for energy saving and industrial applications; [0003] Harrar et al. (J.Electrochem.Soc, 1997,144(6):2032-2044.) reported the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B13/08
Inventor 王庆法章一夫柴静王莅张香文
Owner TIANJIN UNIV
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