CN100362136C - Nitric anhydride electrochemical device and method - Google Patents

Nitric anhydride electrochemical device and method Download PDF

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CN100362136C
CN100362136C CNB2005100148207A CN200510014820A CN100362136C CN 100362136 C CN100362136 C CN 100362136C CN B2005100148207 A CNB2005100148207 A CN B2005100148207A CN 200510014820 A CN200510014820 A CN 200510014820A CN 100362136 C CN100362136 C CN 100362136C
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张香文
王庆法
王莅
苏敏
米镇涛
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Tianjin University
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Abstract

The present invention discloses a device and a method for electrochemically preparing dinitrogen pentoxide, which belongs to the preparation technology of dinitrogen pentoxide. In the device, a membrane is arranged at the center of a sealed cavity; both ends of the cavity at both sides of the membrane are respectively provided with an anode plate and a cathode plate; an electrode plate uses a coating Ti plate on which IrO2, RuO2-IrO2, RuO2-IrO2-TiO2 or Pt is coated; the membrane uses a hydrophobic porous polytetrafluoroethylene membrane. The method comprises the steps of the preparation of an initial electrolyte and the determination of a main operating condition. An electrolyte of an anode chamber is saturated salpeter solution of which the mass concentration of N2O4 is 20%; an electrolyte of a cathode chamber is fresh salpeter solution; under the conditions of electrolytic temperature of 0 to 25 DEG C, electrode voltage of +2.0 V to +10V and current density of 500 Am<-2> to 2000 Am<-2>, the electrolyte of the anode chamber and the electrolyte of the cathode chamber respectively circularly flow at the speed of 20 mL/min to 50 mL/min and 30 mL/min to 60 mL/min by an intermittent operation method; the electrolyte of the anode chamber and the electrolyte of the cathode chamber flow in parallel and circulate. The present invention has the advantages of simple device structure, convenient operation and long electrode life. Compared with the prior art, the current efficiency is increased more than 10%, and the specific energy is reduced 0.86 kWh/kg N2O5.

Description

Nitric anhydride electrochemical device and method
Technical field
The present invention relates to a kind of nitric anhydride electrochemical device and method, belong to the nitrogen pentoxide technology of preparing.
Background technology
Nitration reaction is one of primitive reaction of organic synthesis.Traditional nitrating agent such as nitric acid, there are severe reaction conditions in nitric-sulfuric acid or nitric acid acetic anhydride, shortcomings such as poor selectivity.Anhydrous nitric acid can partly overcome above-mentioned shortcoming as nitrating agent, but its preparation method (circulate a large amount of sulfuric acid or magnesium nitrate carry out salpeter solution dehydration system anhydrous nitric acid) energy consumption and investment are big.N 2O 5Be a kind of very strong selective nitration agent, especially N 2O 5/ organic solution system is as nitrating agent.Many researchers finds to use N 2O 5As nitrating agent carry out organic when nitrated speed of response fast, efficient height and yield height.
GB231546 is first to the N in the Direct Electrochemistry oxidation salpeter solution 2O 4Method is reported.J.ZawadskiZ.Bankowski, Roznicki Chemii, Vol.22 pp233 (1948) makes further research this process.The basic reaction of this method is to be that Pt does that anode, Pb are done negative electrode, porous ceramics is oxidation N in the membranous electrolyzer at electrode 2O 4/ salpeter solution prepares N 2O 5Compare with the method for front, this process does not need chemical dehydration reagent.But do not note control to electrolytic condition.
N 2O 4+2HNO 3→2N 2O 5+2H ++2e -
J E Harrar etc. J Electrochem SocVol.130, pp108-112 (1983) prepares N by adopting control electromotive force technology to above-mentioned Direct Electrochemistry 2O 5Process is improved.Anode adopts IrO 2/ Pt or IrO 2/ Ti, platinum filament is done negative electrode, and barrier film adopts sintered glass or Nafion film, keeps N 2O 4/ HNO 3Electromotive force between solution and the anode is invariable, has improved current efficiency, thereby has reduced the cost of electrochemical process.USP4,432,902 and 4,525,252 and 4,443,308 pairs of these development further describe.But the electromotive force Controlling System more complicated that adopts in this technological process is difficult for amplifying research.
USP6,200,456 Hes J Electrochem SocVol.144, pp 2032-2044 (1997) have described a kind of electrochemical process and have prepared N 2O 5Amplification process, electrode adopts Pt/Nb, Pt-Ir/Nb, IrO 2/ Ti or IrO 2Materials such as/Al, barrier film adopts anion-exchange membrane and PTFE film, and being added with a spot of metal oxide in this PTFE barrier film increases membranous wetting ability.Adopt different diaphragm materials, also inequality in the electrolytic process by membranous transmittance process.The PTFE film has preferable performance in this process.But the influence of PTFE film is not further investigated in the document, and the energy consumption of electrolytic process is also higher relatively.
Summary of the invention
The objective of the invention is to be to provide a kind of nitric anhydride electrochemical device and method, adopt this technology to prepare the nitrogen pentoxide high efficiency, energy consumption is low, and is simple to operate.
The present invention realizes by under the following technical proposals: a kind of nitric anhydride electrochemical device, described device is provided with a barrier film in the central authorities of the cavity of a sealing, two ends at membranous both sides cavity are provided with positive plate and negative plate respectively, barrier film and positive plate constitute the anolyte compartment, and barrier film and negative plate constitute cathode compartment.It is characterized in that it is to be matrix with the titanium material that positive-negative electrode plate adopts matrix material, described matrix material, coating IrO it on 2, RuO 2-IrO 2, RuO 2-IrO 2-TiO 2Or the coating of Pt, thickness 5～70 μ m of coating; In the coating of multicomponent mixture, IrO 2The mass content of component in this coating is 50%～90%; Barrier film adopts hydrophobic porous poly tetrafluoroethylene, and membrane pore size is at 0.002～10.0 μ m, and porosity is 30%～80%, and membrane thicknesses is at 30～2000 μ m.The specific electrode surface of electrolyzer is 30～1000m 2/ m 3, under the condition that guarantees electrolyzer throughput, electrolyzer adopts high specific electrode surface as far as possible.
Above-mentioned hydrophobic porous tetrafluoroethylene membrane pore size is 0.004～2.0 μ m; Porosity is 50%～70%; Thickness is 60～200 μ m.
The coating of above-mentioned positive plate is IrO 2, RuO 2-IrO 2Or RuO 2-IrO 2-TiO 2The negative plate coating is IrO 2, RuO 2-IrO 2Or Pt.
Adopt said apparatus to realize preparing the method for nitrogen pentoxide, its feature comprises following process:
1. the preparation of initial electrolysis liquid feeds N with concentration 98% salpeter solution 2O 4, be mixed with mass concentration and be 20% to saturated anolyte compartment's electrolytic solution; Cathode compartment electrolytic solution is 98% fresh salpeter solution;
2. employing intermittent process, each electrolytic anode and cathode liquor capacity is 2～5 times of tank room volume; Electrolysis temperature is controlled at 0 ℃～25 ℃, and electrode voltage is controlled at+2.0V～+ 10V, current density is controlled at 500Am -2～2000 Am -2Anolyte compartment's electrolytic solution circulates with 30～60mL/min, and cathode compartment electrolytic solution circulates with 20～50mL/min, and anode and cathode electrolytic solution and stream circulation; The N of cathode compartment electrolytic solution in the electrolytic process 2O 4Mass concentration is controlled at below 33% the nearly saturation concentration.
Above-mentioned electrolysis temperature is controlled at 10～20 ℃, and electrode voltage is controlled at+2V～+ 5V, current density is controlled at 700Am -2～1500Am -2, the N of cathode compartment electrolytic solution in the electrolytic process 2O 4Mass concentration is 10%～25%.
The invention has the advantages that the simple in structure of device, easy to operate, compared with prior art, the present invention has adopted the titanium electrode of multi-element metal oxide coating, these metal oxides have electrocatalysis characteristic and lower overpotential preferably in electrolytic process, and erosion resistance is better, and electrode life is long; Hydrophobic porous PTFE barrier film can suppress the water anode diffusion that negative electrode generates in the electrolytic process, thereby compared with prior art, current efficiency improves more than 10% under identical electrolytic condition, and the specific energy of electrolytic process is from 1.6kWh/kgN 2O 5Reduce to 0.74kWh/kgN 2O 5
Description of drawings
Fig. 1 is an apparatus structure synoptic diagram of the present invention.1 for supporting among the figure, and 2 is negative plate, and 3 is cathode compartment, and 4 is the catholyte import, and 5 is barrier film, and 6 is the anolyte compartment, and 7 is the anolyte import, and 8 is positive plate, and 9 are the anolyte outlet, and 10 are the catholyte outlet.
Fig. 2. current density is with electrolysis time change trend curve figure in the electrolytic process of the present invention.
Current density is with initial voltage variation trend curve figure in Fig. 3 electrolytic process of the present invention.
By Fig. 2 and Fig. 3 as can be seen, negative electrode and anodic overpotential are lower, and the resistance of electrolyzer is lower in the electrolytic process, electrolysis under the 2.29V constant voltage, the anode no oxygen produces, electrolysis smooth running under higher current density, thereby adopt this device to carry out electrolysis energy consumption and obviously reduce.
Embodiment
Following embodiment has embodied the process that the present invention describes, but the present invention is not limited to these examples.The material of the electrolyzer key part that process is used and diaphragm material see Table 1 and table 2 respectively.
Table 1
Preparation N 2O 5Each parts material in the process
Assembly Material
Electrolyzer sheet frame metallic support electrode diaphragm PTFE stainless steel IrO 2/Ti、Pt/Ti、RuO 2-IrO 2/ Ti sees Table 2
Pipeline and joint pump and the storage of valve gas-liquid separator are irritated PTFE PTFE﹠ glass glass glass
Table 2
Diaphragm material
The barrier film model Trade(brand)name Production code member or model Producer is provided
GL GD GS BS EXCELLERATOR Separator Gas Diffusion membrane Gore-Tex ionization film PTFE micropore filtering film - Unsitnered D SGT100T100-1 BS01 Gore company of Gore company of Gore company Beijing plastic institute
Embodiment 1
In the anode and cathode storage tank, respectively add 20ml 98% concentrated nitric acid, in the anode storage tank, add N 2O 4Configuration concentration is 25.0%N 2O 4/ HNO 3Solution uses surge pump that it is squeezed into electrolyzer.The effective working area of electrolyzer is 7cm 2, specific electrode surface adopts 100m 2/ m 3, IrO 2/ Ti is an anode, RuO 2-IrO 2/ Ti is negative electrode (mass ratio RuO 2: IrO 2=3: 7), electrode coating thickness is 7 μ m, and barrier film adopts the hydrophobic porous tetrafluoroethylene barrier film of BS, and its contact angle is 128 °, and the BS membrane pore size is 0.1 μ m, porosity 55%, film thickness 0.06mm.Adopt constant voltage operation, service temperature is 10 ℃, applies 2.50V voltage between anode and cathode, and current density is at 800～1200Am -2Between change.Reach maximum value at initial electrolysis 20min to the 60min after-current.Electrolysis is carried out titrimetry to negative and positive level electrolytic solution after 7 hours and is measured each component concentrations in its solution.Experimental result sees Table 3.
Embodiment 2
Adopt method and the electrolytic cell assembly identical with embodiment 1, configuration concentration is 31%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film adopt double-deck BS voided polytetrafluoroethylene film machinery compound, and thickness is about 0.12mm, applies 3.30V voltage at two interpolars, and current density is at 800～1300Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 11 hours, the results are shown in Table 3
Embodiment 3
Adopt method and the electrolytic cell assembly identical with embodiment 1, configuration concentration is 32.5%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film adopt four layers of BS voided polytetrafluoroethylene film machinery compound, and thickness is about 0.24mm, applies 5.50V voltage at two interpolars, and current density is at 1000～1300 Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 8 hours.Direct HNO takes place in overtension in this electrolytic process, anode 3Electrolytic reaction, electrode reaction as shown in the formula:
4HNO 3→2N 2O 5+4H ++O 2+4e -
Although this reaction also generates N 2O 5, but also obtain by product O simultaneously 2, make the current efficiency of electrolytic process reduce, energy consumption increases, simultaneously O 2The also smooth running of influence process of existence.
Embodiment 4
Adopt method and the electrolytic cell assembly identical with embodiment 1, configuration concentration is 32.4%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film adopt untreated BS/GS porous Teflon machinery composite membrane, and GS is the wetting ability barrier film, membrane pore size 1.0 μ m, and porosity 60%, thickness is about 0.15mm, applies 3.79V voltage at two interpolars, and current density is at 900～1500Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 7 hours, the results are shown in Table 3.
The comparative example 5
Adopt method and the electrolytic cell assembly identical with embodiment 4, configuration concentration is 31.9%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film are adopted BS/GS porous Teflon machinery composite membrane, this film before using near saturated N 2O 4/ HNO 3Dipping is 24 hours in the solution, applies 2.1V voltage at two interpolars, and current density is at 900～1200Am -2Between change, current density reaches maximum value at 10min between the 30min, electrolysis was analyzed anode and cathode electrolytic solution after 6 hours, the results are shown in Table 3.
Embodiment 6
Adopt method and the electrolytic cell assembly identical with embodiment 1, configuration concentration is 32.5%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film adopts the hydrophobic porous poly tetrafluoroethylene of GD, and its contact angle is 96 °, membrane pore size 0.1 μ m, porosity 60%, thickness is about 0.10mm, applies 3.32V voltage at two interpolars, and current density is at 1000～1500Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 7.2 hours, the results are shown in Table 3.
Embodiment 7
Adopt method and the electrolytic cell assembly identical with embodiment 5, configuration concentration is 20.3%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film adopts the hydrophilic porous poly tetrafluoroethylene of GL, membrane pore size 0.1 μ m, porosity 60%, thickness is about 0.023mm, applies 2.98V voltage at two interpolars, and current density is at 800～1300Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 8.5 hours, the results are shown in Table 3.
Embodiment 8
Adopt method and the electrolytic cell assembly identical with embodiment 1, configuration concentration is 30.0%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film adopts the hydrophobic porous poly tetrafluoroethylene of BS, and membrane pore size is 0.5 μ m, porosity 60%, film thickness 0.06mm.Apply 2.92V voltage at two interpolars, current density is at 1000～1300Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 7.5 hours, the results are shown in Table 3.
Embodiment 9
Adopt method and the electrolytic cell assembly identical with embodiment 1, configuration concentration is 34.0%N in the anode storage tank 2O 4/ HNO 3Solution, barrier film adopts the hydrophobic porous poly tetrafluoroethylene of BS, and membrane pore size is 1.0 μ m, porosity 60%, film thickness 0.06mm.Apply 2.4V voltage at two interpolars, current density is at 1000～1300Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 5.5 hours, the results are shown in Table 3.
Embodiment 10
Adopt method and the electrolytic cell assembly identical with embodiment 6, anode adopts the Pt/Ti electrode, negative electrode employing RuO 2-IrO 2/ Ti.Configuration concentration is 37.6%N in the anode storage tank 2O 4/ HNO 3Solution applies 3.5V voltage at two interpolars, and current density is at 1000～1400Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 7 hours, the results are shown in Table 3.
Embodiment 11
Adopt method and the electrolytic cell assembly identical with embodiment 6, anode adopts the Pt/Ti electrode, negative electrode employing IrO 2/ Ti.Configuration concentration is 35.4%N in the anode storage tank 2O 4/ HNO 3Solution applies 3.9V voltage at two interpolars, and current density is at 900～1600Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 6.2 hours, the results are shown in Table 3.
Embodiment 12
Adopt method and the electrolytic cell assembly identical, anode employing IrO with embodiment 6 2/ Ti electrode, negative electrode adopts IrO 2/ Ti.Configuration concentration is 36.0%N in the anode storage tank 2O 4/ HNO 3Solution applies 2.7V voltage at two interpolars, and current density is at 900～1600Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 7.2 hours, the results are shown in Table 3.
Embodiment 13
Adopt method and the electrolytic cell assembly identical, anode employing RuO with embodiment 6 2-IrO 2/ Ti electrode, negative electrode adopts IrO 2/ Ti.Configuration concentration is 23.2%N in the anode storage tank 2O 4/ HNO 3Solution applies 2.7V voltage at two interpolars, and current density is at 900～1600Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 7.5 hours, the results are shown in Table 3.
Embodiment 14
Adopt method and the electrolytic cell assembly identical, anode employing RuO with embodiment 6 2-IrO 2/ Ti electrode, negative electrode adopts Pt/Ti.Configuration concentration is 29.3%N in the anode storage tank 2O 4/ HNO 3Solution applies 2.46V voltage at two interpolars, and current density is at 900～1500Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 8 hours, the results are shown in Table 3.
Embodiment 15
Adopt method and the electrolytic cell assembly identical, anode employing IrO with embodiment 6 2/ Ti electrode, negative electrode adopts Pt/Ti.Configuration concentration is 33.1%N in the anode storage tank 2O 4/ HNO 3Solution applies 2.45V voltage at two interpolars, and current density is at 1000～1500Am -2Between change, electrolysis was analyzed anode and cathode electrolytic solution after 8 hours, the results are shown in Table 3.
Electrolytic experiment result under table 3 different condition
Embodiment Initial N 2O 4，％ Anolyte, wt% Yield, % Current efficiency, % Specific energy, kWh/ kgN 2O 5
N 2O 5 N 2O 4
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 24.95 31.00 32.50 32.37 31.9 32.46 20.25 29.9 34.14 37.6 35.4 36.0 23.2 29.3 33.1 30.03 26.82 23.40 25.03 24.61 35.25 17.94 20.87 16.62 31.55 25.66 35.87 20.63 37.61 28.63 7.94 14.08 4.59 11.08 11.8 13.11 8.79 10.93 14.72 14.09 16.34 10.66 6.86 14.63 12.35 44.44 39.23 26.73 35.10 29.83 45.33 47.31 30.81 20.27 38.95 36.32 47.70 47.32 56.23 44.25 83.70 48.45 37.10 60.57 62..36 80.22 54.26 40.05 42.53 79.77 86.88 78.49 49.30 89.23 67.33 0.74 1.71 3.56 1.59 0.80 1.05 1.31 1.81 1.40 1.11 1.18 0.86 1.47 0.72 0.92

Claims (5)

1. nitric anhydride electrochemical device, described device is provided with a barrier film in the central authorities of the cavity of a sealing, two ends at membranous both sides cavity are provided with positive plate and negative plate respectively, barrier film and positive plate constitute the anolyte compartment, barrier film and negative plate constitute cathode compartment, it is characterized in that it is to be matrix with the titanium material that positive-negative electrode plate adopts matrix material, described matrix material, coating IrO it on 2, RuO 2-IrO 2, RuO 2-IrO 2-TiO 2Or the coating of Pt, thickness 5～70 μ m of coating; In the coating of multicomponent mixture, IrO 2The mass content of component in this coating is 50%～90%; Barrier film adopts hydrophobic porous poly tetrafluoroethylene, and membrane pore size is at 0.002～10.0 μ m, and porosity is 30%～80%, and membrane thicknesses is 30～2000 μ m; The specific electrode surface of electrolyzer is 30～1000m 2/ m 3, under the condition that guarantees electrolyzer throughput, electrolyzer adopts high specific electrode surface as far as possible.
2. by the described nitric anhydride electrochemical device of claim 1, it is characterized in that membrane pore size is 0.004～2.0 μ m, porosity is 50%～70%, and membranous thickness is 60～200 μ m.
3. by the described nitric anhydride electrochemical device of claim 1, the coating that it is characterized in that positive plate is IrO 2, RuO 2-IrO 2Or RuO 2-IrO 2-TiO 2The negative plate coating is IrO 2, RuO 2-IrO 2Or Pt.
4. a device that adopts claim 1 is realized the method for nitric anhydride electrochemical, it is characterized in that comprising following process:
1) preparation of initial electrolysis liquid feeds N with concentration 98% salpeter solution 2O 4, be mixed with mass concentration and be 20% to saturated anolyte compartment's electrolytic solution; Cathode compartment electrolytic solution is 98% fresh salpeter solution;
2) adopt intermittent process, each electrolytic anode and cathode liquor capacity is 2～5 times of tank room volume; Electrolysis temperature is controlled at 0 ℃～25 ℃, and electrode voltage is controlled at+2.0V～+ 10V, current density is controlled at 500Am -2～2000Am -2, anolyte compartment's electrolytic solution circulates with 30～60mL/min, and cathode compartment electrolytic solution circulates with 20～50mL/min, and anode and cathode electrolytic solution and stream circulation; The N of cathode compartment electrolytic solution in the electrolytic process 2O 4Mass concentration is controlled at below 33% the nearly saturation concentration.
5. by the method for the described realization nitric anhydride electrochemical of claim 4, it is characterized in that electrolysis temperature is controlled at 10～20 ℃, electrode voltage is controlled at+2V～+ 5V, current density is controlled at 700Am -2～1500Am -2, the N of cathode compartment electrolytic solution in the electrolytic process 2O 4Mass concentration is 10%～25%.
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