CN102173480A - Method for preparing two-phase porous lead dioxide composite electrode - Google Patents
Method for preparing two-phase porous lead dioxide composite electrode Download PDFInfo
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- CN102173480A CN102173480A CN 201110022256 CN201110022256A CN102173480A CN 102173480 A CN102173480 A CN 102173480A CN 201110022256 CN201110022256 CN 201110022256 CN 201110022256 A CN201110022256 A CN 201110022256A CN 102173480 A CN102173480 A CN 102173480A
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- phase porous
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- YADSGOSSYOOKMP-UHFFFAOYSA-N dioxolead Chemical compound O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title abstract description 16
- 239000002131 composite material Substances 0.000 title abstract 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000002142 lead-calcium alloy Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000001117 sulphuric acid Substances 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000006056 electrooxidation reaction Methods 0.000 claims description 5
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 5
- 238000005554 pickling Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 235000012054 meals Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000011505 plaster Substances 0.000 claims 2
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 238000004065 wastewater treatment Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 239000003292 glue Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 16
- 238000004043 dyeing Methods 0.000 description 14
- 239000011159 matrix material Substances 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a method for preparing a two-phase porous lead dioxide composite electrode, which comprises the following steps of: shearing preprocessed active carbon fibrofelt to have a size which is the same as that of the two-phase porous lead dioxide electrode; and bonding the fibrofelt on the two-phase porous lead dioxide electrode prepared on both sides of a lead calcium alloy net which is subjected to compacting, drying and electrochemical oxidizing and of which the surface is coated with paste lead powder by using conducting glue to obtain the two-phase porous lead dioxide composite electrode. In the method, the active carbon fibrofelt is introduced, and the high adsorbability of the active carbon fibrofelt and the high catalytic activity of the lead dioxide powder porous electrode are combined to realize the synergistic effect of gathering-electro-catalytic oxidation, enhance the catalytic activity and improve oxidizability. In addition, the active carbon fibrofelt has excellent electrical conductivity, so energy consumption for wastewater treatment is reduced, and the method for preparing the lead dioxide electrode is easy to operate, stable in the performance of the electrode and high in efficiency of wastewater treatment.
Description
Technical field
The present invention relates to technical field of waste water processing, be specifically related to a kind of preparation method of two-phase porous lead dioxide combined electrode.
Background technology
Dyeing waste water has characteristics such as organic concentration height, colourity height, complicated component, biodegradability difference, and modern dye species is more and more, and develop towards anti-photodissociation, anti-oxidant, biorefractory direction, the treatment of dyeing wastewater difficulty is strengthened, so dyeing waste water is emphasis and difficult point in the Industrial Wastewater Treatment always.At present, still do not have the improvement technology with universality, its governing problem is still a global difficult problem.Although there is lot of advantages in electrochemical method, at present in the middle of the processing of difficult for biological degradation organic waste water, still be subjected to the restriction of electrode materials, higher factors such as energy consumption.
At present, generally adopt titanium-base PbO
2Electrode, i.e. PbO
2/ Ti electrode, electrochemical plating are used in its preparation mostly, and this technology for preparing electrode exists titanium matrix pretreatment procedure than problems such as difficult control, electrode performance are stable inadequately, fall short of work-ing life.Therefore, generally plate the middle layer in the process of preparation electrode earlier to suppress passivation, but this process has increased electrode cost of manufacture and process complexity, and is difficult to fundamentally solve the problem of passivation of matrix, also is the not high problem of processing efficiency that causes using this kind electrode pair dyeing waste water.
Based on above reason, invent the making method of the lead dioxide electrode that a kind of easy to implement, electrode performance is stable, waste water treatment efficiency is high, be assistant officer's problem to be solved in the present technique field.
Summary of the invention
For overcoming deficiency of the prior art, the object of the present invention is to provide a kind of preparation method of two-phase porous lead dioxide combined electrode, stablize, handle the not high enough problem of waste water efficient inadequately with the difficult control of electrode operation, the electrode performance that solve treatment of dyeing and printing in the prior art.
For reaching above-mentioned technical purpose, the technical solution used in the present invention is: a kind of preparation method of two-phase porous lead dioxide combined electrode: the pretreated active carbon fibrefelt is cut into small pieces, stick to the both sides of two-phase porous lead dioxide electrode with conductive resin, promptly make two-phase porous lead dioxide combined electrode.
The pretreatment process of wherein said activated carbon fiber felt is as follows:
After activated carbon fiber is successively passed through pre-treatment step such as alkali cleaning, pickling, poach,, standby in drying in the temperature more than 100 ℃.
Preferably, what the alkali cleaning step was used is that concentration ratio is 1: 1 a ammoniacal liquor, and what acid pickling step used is that concentration ratio is 1: 1 HNO
3Or HCl, poach step are with distillation poach 2h.
The preparation method of wherein said two-phase voluminous powder plumbic oxide combined electrode is as follows:
(a) preparation of lead powder: lead pig is made shot or lead earlier, grind in the ball mill of packing into, and air blast is oxidized to lead powder.The lead powder that makes is the two-phase body particle meal of the metallic lead of surface coverage one deck plumbous oxide then, and the oxidisability of lead powder is generally 65%～80%.
(b) preparation of two-phase porous lead dioxide electrode: at first in an amount of lead powder, add distilled water, the add-on of distilled water is to add 3-10ml in every 100g lead powder, the sulphuric acid soln vitriolic add-on that adds density again and be 1.14～1.35g/L is to add 7.5-18.4mL in every 100g lead powder, lead powder is in harmonious proportion to paste, it is online that this lotion is spread upon lead-calcium alloy, promptly gets the two-phase porous lead dioxide electrode through compacting, oven dry, electrochemical oxidation.
Preferably, the electrochemical oxidation in the described step (b) is to finish by the following method: it is 1.00～1.10g/cm that the electrode after compacting, oven dry places density
3Sulphuric acid soln in, be anode, be equipped with negative electrode stable in sulphuric acid soln that with this electrode the feeding current density is 10～20mA/cm
2Galvanic current, when electrode surface become brown stop the energising; Take out above-mentioned electrode, use distilled water flushing, oven dry promptly gets powder porous lead dioxide electrode about 30～50 ℃.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. kind electrode belongs to the two-phase porous electrode, and the real surface of electrode is long-pending to be higher than ti-supported lead dioxide electric pole far away, so reaction area increases greatly;
2. introduce the activated carbon fiber felt, the strong characterization of adsorption of activated carbon fiber felt and the high catalytic activity of two-phase porous lead dioxide electrode are combined, realized the synergistic effect of enrichment-catalytic oxidation, catalytic activity strengthens greatly, and oxidation capacity improves greatly; Because the activated carbon fiber felt has good electrical conductivity, the energy consumption of therefore handling waste water reduces greatly in addition.
3. adopt the lead-calcium alloy matrix to replace the titanium matrix, avoided the matrix problem of passivation;
4. making processes is comparatively simple, easy to implement;
5. compare with conventional treatment method of printing and dying wastewater, this method can not produce excess sludge.
6. adopt the two-phase voluminous powder plumbic oxide combined electrode of the present invention's preparation effective to treatment of dyeing wastewater.
Embodiment
The first step, the preparation of lead powder:
Lead pig is made shot or lead earlier, grind in the ball mill of packing into, and air blast is oxidized to lead powder.
Second step, the preparation of two-phase porous lead dioxide electrode:
Add distilled water earlier in the above-mentioned lead powder for preparing, add the sulphuric acid soln that density is 1.14g/L again, be in harmonious proportion to thick, wherein lead powder, water and vitriolic ratio are 100g: 5mL: 10mL; It is that the lead-calcium alloy of 3cm * 3cm is online that this lotion is spread upon area, promptly gets the two-phase porous lead dioxide electrode through compacting, oven dry, electrochemical oxidation.
The 3rd step, the pre-treatment of activated carbon fiber felt:
The activated carbon fiber felt successively passes through alkali cleaning (with 1: 1 ammoniacal liquor), pickling (with 1: 1 HNO
3Or HCl), after the pre-treatment step such as poach (distillation poach 2h), in drying in the temperature more than 100 ℃, standby.
The 4th step, the preparation of two-phase porous lead dioxide combined electrode:
The pretreated active carbon fibrefelt is cut into the square of 3cm * 3cm, sticks to the both sides of prepared two-phase porous lead dioxide electrode of second step, promptly make two-phase porous lead dioxide combined electrode of the present invention with conductive resin.
Two-phase porous lead dioxide combined electrode of the present invention is tested the treatment effect of dyeing waste water:
Dyeing waste water is taken from Suzhou printing and dyeing mill, after testing: pH=8.78, TOC=4.81g/L.With this electrode is anode, and two stainless steel electrodes lay respectively at this anodic both sides.Control current density is 20mA/cm
2, temperature is 40 ℃, adopts magnetic agitation, and above-mentioned dyeing waste water dilution is degraded for ten times, adopts German Multi-N/C 3100 analysis-e/or determining TOC.
Table 1 two-phase porous lead dioxide of the present invention combined electrode is to the degradation effect of dyeing waste water
As can be seen from Table 1, two-phase porous lead dioxide combined electrode of the present invention is after the TOC clearance has reached 51.4%, 8 hour in 1 hour, and the TOC clearance has reached 86.3%.Groove is pressed in the whole degradation process comparatively stable, about average out to 3.5V.Relatively the color of dyeing waste water can be found before and after the degraded, is black-and-blue before the degraded, and it is transparent to become colorless after the degraded.
In order to compare with simple two-phase porous lead dioxide electrode, the contriver adopts simple two-phase porous lead dioxide electrode that above-mentioned dyeing waste water is degraded again.Test condition is the same, and the result is as shown in table 2.
The simple two-phase porous lead dioxide electrode of table 2 is to the degradation effect of dyeing waste water
As can be seen from Table 2, simple two-phase porous lead dioxide electrode was 79% to the TOC clearance in 8 hours afterwards, be lower than the two-phase porous lead dioxide combined electrode in the table 1, and average groove pressure is higher than the groove pressure of the two-phase porous lead dioxide combined electrode in the table 1 far away for about 12V.
Claims (7)
1. the preparation method of a two-phase porous lead dioxide combined electrode is characterized in that, comprises following steps:
The preparation of step 1) lead plaster: add distilled water in lead powder, the add-on of described distilled water is to add 3-10ml in every 100g lead powder; Add the sulphuric acid soln that density is 1.14～1.35g/L again, described vitriolic add-on is to add 7.5-18.4mL in every 100g lead powder;
Step 2) preparation of two-phase porous lead dioxide electrode: will the lead plaster after step 1) is handled to spread upon lead-calcium alloy online, promptly get the two-phase porous lead dioxide electrode through compacting, oven dry, electrochemical oxidation;
The pre-treatment of step 3) activated carbon fiber felt: after the activated carbon fiber felt successively being passed through steps such as alkali cleaning, pickling and poach, in 100 ℃ of-150 ℃ of temperature, dry, get the activated carbon fiber felt, standby;
The preparation of step 4) two-phase porous lead dioxide combined electrode: the pretreated active carbon fibrefelt is cut into small pieces, sticks to the both sides of the two-phase porous lead dioxide electrode that makes through step 3), promptly make two-phase porous lead dioxide combined electrode with conductive resin.
2. the preparation method of two-phase porous lead dioxide combined electrode according to claim 1, it is characterized in that, lead powder described in the step 1) is made by following steps: lead pig is made shot or lead earlier, grind in the ball mill of packing into, and air blast is oxidized to lead powder.
3. the preparation method of two-phase porous lead dioxide combined electrode according to claim 2 is characterized in that, described lead powder is the two-phase body particle meal that surface coverage has one deck plumbous oxide, and the oxidisability of lead powder is 65%～80%.
4. the preparation method of two-phase porous lead dioxide combined electrode according to claim 1 is characterized in that, described step 2) in the area of lead-calcium alloy net be 3cm * 3cm.
5. the preparation method of two-phase porous lead dioxide combined electrode according to claim 1, it is characterized in that, the concrete steps of the electrochemical oxidation described step 2) are: will place density through the electrode after compacting, the oven dry is the sulphuric acid soln of 1.14～1.35g/L, be anode, be equipped with negative electrode stable in sulphuric acid soln that with this electrode the feeding current density is 10mA/cm
2～20mA/cm
2Galvanic current, when electrode surface become brown stop the energising; Take out above-mentioned electrode, use distilled water flushing, oven dry promptly gets the two-phase porous lead dioxide electrode under 30～50 ℃ of temperature.
6. the preparation method of two-phase porous lead dioxide combined electrode according to claim 1 is characterized in that, use in the alkali cleaning step in the described step 3) be concentration ratio be 1: 1 ammoniacal liquor as alkali, what use in the acid pickling step is that concentration ratio is 1: 1 HNO
3Or HCl is as acid, and the poach step is for distillation poach 2 hours.
7. the preparation method of two-phase porous lead dioxide combined electrode according to claim 1 is characterized in that, in the described step 4), the fritter that described activated carbon fiber felt is cut into is the square of area 3cm * 3cm.
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| CN 201110022256 CN102173480B (en) | 2011-01-20 | 2011-01-20 | Method for preparing two-phase porous lead dioxide composite electrode |
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| CN 201110022256 CN102173480B (en) | 2011-01-20 | 2011-01-20 | Method for preparing two-phase porous lead dioxide composite electrode |
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| CN102173480B CN102173480B (en) | 2013-02-06 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103116046A (en) * | 2012-12-12 | 2013-05-22 | 上海电气钠硫储能技术有限公司 | Preparation method for absorbing mixed fused salt carbon felt electrodes |
| CN111048777A (en) * | 2019-12-13 | 2020-04-21 | 浙江天能动力能源有限公司 | High-porosity EVF series lead storage battery positive electrode lead plaster and plaster mixing method thereof |
| CN112159987A (en) * | 2020-09-03 | 2021-01-01 | 广东臻鼎环境科技有限公司 | Sandwich structure composite lead electrode and preparation method thereof |
| CN112226785A (en) * | 2020-09-03 | 2021-01-15 | 广东臻鼎环境科技有限公司 | Foam copper-based composite lead electrode and preparation method thereof |
| CN112226786A (en) * | 2020-09-03 | 2021-01-15 | 广东臻鼎环境科技有限公司 | Composite lead dioxide electrode and preparation method thereof |
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| JP2005025955A (en) * | 2003-06-30 | 2005-01-27 | Furukawa Battery Co Ltd:The | Lead acid battery and its manufacturing method |
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| CN101555051A (en) * | 2009-05-05 | 2009-10-14 | 苏州科技学院 | Production method for powder porous lead dioxide electrode used for treating organics in water |
-
2011
- 2011-01-20 CN CN 201110022256 patent/CN102173480B/en not_active Expired - Fee Related
Patent Citations (4)
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|---|---|---|---|---|
| JPH05166504A (en) * | 1991-12-11 | 1993-07-02 | Yuasa Corp | Manufacture of lead-acid battery positive electrode plate |
| JP2005025955A (en) * | 2003-06-30 | 2005-01-27 | Furukawa Battery Co Ltd:The | Lead acid battery and its manufacturing method |
| CN101417831A (en) * | 2008-11-11 | 2009-04-29 | 北京师范大学 | Novel ti-supported lead dioxide electric pole and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103116046A (en) * | 2012-12-12 | 2013-05-22 | 上海电气钠硫储能技术有限公司 | Preparation method for absorbing mixed fused salt carbon felt electrodes |
| CN103116046B (en) * | 2012-12-12 | 2015-03-25 | 上海电气钠硫储能技术有限公司 | Preparation method for absorbing mixed fused salt carbon felt electrodes |
| CN111048777A (en) * | 2019-12-13 | 2020-04-21 | 浙江天能动力能源有限公司 | High-porosity EVF series lead storage battery positive electrode lead plaster and plaster mixing method thereof |
| CN112159987A (en) * | 2020-09-03 | 2021-01-01 | 广东臻鼎环境科技有限公司 | Sandwich structure composite lead electrode and preparation method thereof |
| CN112226785A (en) * | 2020-09-03 | 2021-01-15 | 广东臻鼎环境科技有限公司 | Foam copper-based composite lead electrode and preparation method thereof |
| CN112226786A (en) * | 2020-09-03 | 2021-01-15 | 广东臻鼎环境科技有限公司 | Composite lead dioxide electrode and preparation method thereof |
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Address after: 215011 No. 1701 Binhe Road, Jiangsu, Suzhou Patentee after: SUZHOU University OF SCIENCE AND TECHNOLOGY Address before: 215011 No. 1701 Binhe Road, Jiangsu, Suzhou Patentee before: University of Science and Technology of Suzhou |
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Effective date of registration: 20191212 Address after: 215000 station 1802-6, Yueliangwan International Conference Center, No. 9, Cuiwei street, Suzhou Industrial Park, Suzhou City, Jiangsu Province (cluster registration) Patentee after: Jiangsu Yuyi environmental protection engineering equipment Co.,Ltd. Address before: 215011 No. 1701 Binhe Road, Jiangsu, Suzhou Patentee before: Suzhou University of Science and Technology |
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Granted publication date: 20130206 |