CN108301019A - A kind of technology for preparing electrode with long service life - Google Patents
A kind of technology for preparing electrode with long service life Download PDFInfo
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
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Abstract
The invention discloses a kind of technology for preparing electrode with long service life, including sandblasting polishing step：Electrode matrix is taken, electrode matrix is placed in sand-blasting machine, setting blasting pressure is 0.5 1MPa, and sandblasting angle is 45 90 °, and sand grains flow is 5 10Kg/h, and blast time is 2 6min, and the roughness of coordination electrode matrix is 4 10 μm.Electrode acquired in technology for preparing electrode provided by the present invention has to be increased with coating binding force, the advantages that specific surface area of electrode increases, electric conductivity enhances, chlorine evolution potential reduces, the reinforcing life time is long, to realize the advantages such as electrolytic efficiency raising in electrolytic process, electrolytic cell calorific value reduction, operation energy consumption reduction, electrode life length.
Description
Technical field
The present invention relates to electrode fabrication field more particularly to a kind of technology for preparing electrode with long service life.
Background technology
With constantly contaminated and water resource the continuous shortage of water resource on the earth, disinfection water process seems more and more heavier
It wants；Cholorination is current the most widely used water sterilization method, is played an important role in terms of pre- waterproof spreads the disease.
Chlorine or hypochlorite (such as NaClO) are added into water, can generally generate hypochlorous acid (HClO) and hydrochloric acid (HCl).Sodium hypochlorite
Generator generates the sodium hypochlorite solution of low concentration, its Disinfection Effect is good, and it is accurate to add, and safe operation is easy to use, is easy to store up
It deposits, to environment nonhazardous, does not generate second of pollution, there is advantage very much.
Electrolytic cell is the Workplace of liquor natrii hypochloritis, and Ti electrode is the core component of electrolytic cell.The analysis chlorine of Ti electrode
Electrolytic efficiency, electrolysis energy consumption and the operating cost etc. that efficiency and service life produce sodium hypochlorite play vital work
With.
The patent of Patent No. 201110137977.4《Anode for electrolysis and preparation method thereof》It provides a kind of for electricity
The Ti electrode preparation method of solution production chlorine, but the Ti electrode disclosed in the invention has the following defects：Titanium base specific surface area is low,
The shortcomings of chlorine evolution potential is high, Titanium base and coating binding force are poor, electric conductivity is poor, service life is short, eventually leads to sodium hypochlorite
The consequences such as electrolytic efficiency declines in generator electrolytic process, electrolytic cell calorific value is big, operation energy consumption improves.
Invention content
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of electrodes with long service life to prepare work
Skill is polished this crucial processing step in preparation process by sandblasting, to increase the specific surface area of electrode matrix, increase
Big electric conductivity, while ensure that electrode matrix has excellent binding force with coating.
The purpose of the present invention adopts the following technical scheme that realization：
A kind of technology for preparing electrode with long service life, including sandblasting polishing step：Electrode matrix is taken, by the electrode base
Body is placed in sand-blasting machine, and setting blasting pressure is 0.5-1MPa, and sandblasting angle is 45-90 °, and sand grains flow is 5-10Kg/h, spray
The sand time is 2-6min, and the roughness of coordination electrode matrix is 4-10 μm.
Further, sand grains type is one kind in corundum, silicon carbide sand and aluminum oxide sand or arbitrary combination.
Further, the granularity of sand grains is 30-75 mesh.
Further, further include cutting step：Electrode base material is taken, the electrode base material is cut into preset shape, is obtained
The electrode matrix of acquisition is then carried out sandblasting polishing by electrode matrix；
Alkali cleaning deoiling step：The electrode matrix is placed in aqueous slkali after sandblasting is polished and carries out ultrasonic activation, with
It takes out and is cleaned up with clear water afterwards；
Pickling etching step：The electrode matrix is placed in acid solution and heats and boil, then take after alkali cleaning oil removing
Go out and is cleaned up with clear water；
Coating sintering step：The electrode matrix after overpickling etches, be repeated successively noble metal-coating coating solution,
Drying and sintering processes.
Further, in the cutting step, the electrode base material is the metallic plate that thickness is 1-2mm, is cut using line
It cuts or the electrode base material is cut into preset shape by laser cutting method.
Further, in the alkali cleaning deoiling step, the electrode matrix is placed in mass fraction after sandblasting is polished
For in the sodium hydroxide solution of 6-12%, temperature is constant 20- is vibrated in 70-90 DEG C, the ultrasonic wave that power is 1000-2000W
40min is clean wash with distilled water after taking-up.
Further, in the pickling etching step, the electrode matrix is placed in mass fraction after alkali cleaning oil removing
It is clean wash with distilled water after taking-up in the sulfuric acid solution of 5-12%, to boil 1-3h.
Further, in the coating sintering step, the number that coating, drying and sintering processes are repeated is 20-
30 times；Drying temperature is 110-180 DEG C, drying time 10-20min；Sintering temperature is 420-480 DEG C, sintering time 10-
20min。
Further, further include high-temperature annealing step：The electrode matrix carries out high annealing after sandblasting is polished,
The temperature of high annealing is 600-1000 DEG C, soaking time 1-3h, and the flatness of coordination electrode matrix is 0.1-0.15mm.
Further, further include the more flat step of high temperature：The electrode matrix carries out high temperature and relatively puts down after coating sintering,
The more flat temperature of high temperature is 420-480 DEG C, soaking time 1-3h, and the flatness of coordination electrode matrix is 0.1-0.2mm.
Further, the sand-blasting machine is suction-type dry blasting machine.
Further, the electrode matrix is Titanium base.
Compared with prior art, the beneficial effects of the present invention are：
Technology for preparing electrode with long service life provided by the present invention, electrode matrix pass through sandblasting grinding process, and tight
The technological parameter of lattice control sandblasting bruting process so that the electrode base sheet of acquisition has the advantages that following notable：
1) oxide layer on electrode matrix surface can be removed, exposes metal layer, increase electric conductivity；
2) smooth electrode matrix can be polished into uniform extra coarse face, increase the specific surface area of electrode matrix, increased
Add electrode reaction effective area, improves electrolytic efficiency；
3) the electrode matrix surface of certain extra coarse degree, can form extremely strong snap-in force with noble coatings, effectively prevent
Electrolytic process floating coat falls off, and increases electrode life.
Specific implementation mode
In the following, in conjunction with specific implementation mode, the present invention is described further, it should be noted that is do not collided
Under the premise of, new embodiment can be formed between various embodiments described below or between each technical characteristic in any combination.
A kind of technology for preparing electrode with long service life, including sandblasting polishing step：Electrode matrix is taken, electrode matrix is set
In sand-blasting machine, setting blasting pressure is 0.5-1MPa, and sandblasting angle is 45-90 °, and sand grains flow is 5-10Kg/h, when sandblasting
Between be 2-6min, the roughness of coordination electrode matrix is 4-10 μm.
As preferred embodiment, sand grains type is one kind or arbitrary in corundum, silicon carbide sand and aluminum oxide sand
Combination.
As preferred embodiment, the granularity of sand grains is 30-75 mesh.
Further include cutting step as preferred embodiment：Electrode base material is taken, electrode base material is cut into default shape
Shape obtains electrode matrix, and the electrode matrix of acquisition is then carried out sandblasting polishing；
Alkali cleaning deoiling step：Electrode matrix is placed in aqueous slkali after sandblasting is polished and carries out ultrasonic activation, then take
Go out and is cleaned up with clear water；
Pickling etching step：Electrode matrix is placed in acid solution and heats and boil after alkali cleaning oil removing, then takes out simultaneously
It is cleaned up with clear water；
Coating sintering step：Noble metal-coating coating solution, drying is repeated after overpickling etches in electrode matrix successively
And sintering processes.
As preferred embodiment, in cutting step, electrode base material is the metallic plate that thickness is 1-2mm, using line
Electrode base material is cut into preset shape by cutting or laser cutting method.
As preferred embodiment, in alkali cleaning deoiling step, electrode matrix is placed in quality point after sandblasting is polished
Number is that temperature is constant to be vibrated in 70-90 DEG C, the ultrasonic wave that power is 1000-2000W in the sodium hydroxide solution of 6-12%
20-40min is clean wash with distilled water after taking-up.
As preferred embodiment, in pickling etching step, electrode matrix is placed in quality point after alkali cleaning oil removing
Number is to boil 1-3h in the sulfuric acid solution of 5-12%, clean wash with distilled water after taking-up.
As preferred embodiment, in coating sintering step, the number of coating, drying and sintering processes is repeated
It is 20-30 times；Drying temperature is 110-180 DEG C, drying time 10-20min；Sintering temperature is 420-480 DEG C, sintering time
For 10-20min.
Further include high-temperature annealing step as preferred embodiment：Electrode matrix carries out high temperature after sandblasting is polished
The temperature of annealing, high annealing is 600-1000 DEG C, soaking time 1-3h, and the flatness of coordination electrode matrix is 0.1-
0.15mm。
Electrode matrix carries out the relatively flat processing of high annealing after sandblasting polishing, on the one hand can will be generated in sandblasting procedures
Flexural deformation it is relatively flat, the flatness of electrode matrix is effectively ensured, to ensure to apply when ensureing subsequent coated noble coatings liquid
The uniformity of layer；On the other hand the texture that electrode matrix can be refined, goes de-stress, electrode matrix is become crisp from toughness
Property, reduce the deformation of generation of the subsequent electrode in sintering process.
Further include the more flat step of high temperature as preferred embodiment：Electrode matrix carries out high temperature after coating sintering
Relatively flat, the more flat temperature of high temperature is 420-480 DEG C, soaking time 1-3h, and the flatness of coordination electrode matrix is 0.1-
0.2mm。
Electrode matrix carries out the relatively flat processing of high temperature after carrying out coating sintering repeatedly, can effectively ensure that the flatness of electrode,
So that electrode group is easier for installation, electrode spacing more stable and uniform, so that electrolytic cell calorific value subtracts in electrolytic process
Small, current efficiency improves, operation energy consumption reduces.
As preferred embodiment, the sand-blasting machine is suction-type dry blasting machine.
As preferred embodiment, electrode matrix is Titanium base.
The technology for preparing electrode with long service life that the embodiment of the present invention is provided is applicable in but is not limited to hypochlorite production
With the preparation of analysis chlorine Ti electrode, electrode matrix passes through sandblasting grinding process, and stringent control sandblasting bruting process in preparation process
Technological parameter, to increase the specific surface area of electrode matrix, increase electric conductivity, at the same ensure that electrode matrix with apply
Layer has excellent binding force.Specifically it is discussed below：
1) oxide layer on electrode matrix surface can be removed, exposes metal layer, increase electric conductivity；
2) smooth electrode matrix can be polished into uniform extra coarse face, increase the specific surface area of electrode matrix, increased
Add electrode reaction effective area, improves electrolytic efficiency；
3) the electrode matrix surface of certain extra coarse degree, can form extremely strong snap-in force with noble coatings, effectively prevent
Electrolytic process floating coat falls off, and increases electrode life.
It is specific embodiment of the present invention below, used raw material, equipment etc. remove special limit in the following embodiments
It can be obtained by buying pattern outside fixed.
Embodiment 1：
A kind of technology for preparing electrode with long service life, including：
Cutting step：It is the titanium plate of 1.0mm as titanium-base to select thickness, using line cutting technology by titanium-base according to figure
Paper cutting processing；
Sandblasting polishing step：By titanium-base in suction-type dry blasting machine sandblasting grinding process, blasting pressure 0.5MPa,
Sand grains type be corundum, grit size be 30 mesh, sandblasting angle be 45 °, sand grains flow be 5Kg/h, blast time 2min,
The roughness for controlling titanium-base is 4 μm；
High-temperature annealing step：Titanium-base after sandblasting is carried out to the relatively flat processing of high annealing, high annealing temperature in fixture
Degree is 600 DEG C, soaking time 1h, and guarantee titanium-based plate flatness is 0.1mm；
Alkali cleaning deoiling step：Titanium-base is subjected to alkali cleaning oil removal treatment, titanium-base is placed in the hydrogen-oxygen that mass fraction is 6%
Change in sodium solution, temperature is constant at 70 DEG C, and power is the ultrasonic activation 20min of 1000W, is done wash with distilled water after taking-up
Only；
Pickling etching step：Titanium base is subjected to pickling etching process, the titanium-base after alkali cleaning, which is placed in mass fraction, is
In 5% sulfuric acid solution, 1h is boiled, it is clean wash with distilled water after taking-up；
Coating sintering step：The titanium-base uniformly mixed noble coatings solution being coated in after pickling etching process
On, it coats, dry, sintering processes repeatedly, the number of occurrence is 20 times；Drying temperature is 110 DEG C, drying time 10min；Sintering
Temperature is 420 DEG C, sintering time 10min.
The more flat step of high temperature：The Ti electrode that coating sintering is completed is subjected to the relatively flat processing of high temperature in fixture, high temperature is relatively flat
Temperature is 420 DEG C, soaking time 1h, and guarantee titanium-based plate flatness is 0.1mm.
Embodiment 2：
A kind of technology for preparing electrode with long service life, including：
Cutting step：It is the titanium plate of 1.5mm as titanium-base to select thickness, using line cutting technology by titanium-base according to figure
Paper cutting processing；
Sandblasting polishing step：By titanium-base in suction-type dry blasting machine sandblasting grinding process, blasting pressure 0.7MPa,
Sand grains type is silicon carbide sand, and grit size is 60 mesh, and sandblasting angle is 60 °, and sand grains flow is 7Kg/h, and blast time is
4min, the roughness for controlling titanium-base are 6 μm；
High-temperature annealing step：Titanium-base after sandblasting is carried out to the relatively flat processing of high annealing, high annealing temperature in fixture
Degree is 800 DEG C, soaking time 1.5h, and guarantee titanium-based plate flatness is 0.12mm；
Alkali cleaning deoiling step：Titanium-base is subjected to alkali cleaning oil removal treatment, titanium-base is placed in the hydrogen-oxygen that mass fraction is 8%
Change in sodium solution, temperature is constant at 80 DEG C, and power is the ultrasonic activation 25min of 1500W, is done wash with distilled water after taking-up
Only；
Pickling etching step：Titanium base is subjected to pickling etching process, the titanium-base after alkali cleaning, which is placed in mass fraction, is
In 8% sulfuric acid solution, 2h is boiled, it is clean wash with distilled water after taking-up；
Coating sintering step：The titanium-base uniformly mixed noble coatings solution being coated in after pickling etching process
On, it coats, dry, sintering processes repeatedly, the number of occurrence is 25 times；Drying temperature is 150 DEG C, drying time 15min；Sintering
Temperature is 450 DEG C, sintering time 15min；
The more flat step of high temperature：The Ti electrode that coating sintering is completed is subjected to the relatively flat processing of high temperature in fixture, high temperature is relatively flat
Temperature is 450 DEG C, soaking time 2h, and guarantee titanium-based plate flatness is 0.15mm.
Embodiment 3：
A kind of technology for preparing electrode with long service life, including：
Cutting step：It is the titanium plate of 2.0mm as titanium-base to select thickness, using laser cutting technique by titanium-base according to
Drawing cutting processing；
Sandblasting polishing step：By titanium-base in suction-type dry blasting machine sandblasting grinding process, blasting pressure 1.0MPa,
Sand grains type is aluminum oxide sand, and grit size is 75 mesh, and sandblasting angle is 90 °, and sand grains flow is 10Kg/h, and blast time is
6min, the roughness for controlling titanium-base are 10 μm；
High-temperature annealing step：Titanium-base after sandblasting is carried out to the relatively flat processing of high annealing, high annealing temperature in fixture
Degree is 1000 DEG C, soaking time 2.0h, and guarantee titanium-based plate flatness is 0.15mm；
Alkali cleaning deoiling step：Titanium-base is subjected to alkali cleaning oil removal treatment, titanium-base is placed in the hydrogen-oxygen that mass fraction is 8%
Change in sodium solution, temperature is constant at 90 DEG C, and power is the ultrasonic activation 30min of 2000W, is done wash with distilled water after taking-up
Only；
Pickling etching step：Titanium base is subjected to pickling etching process, the titanium-base after alkali cleaning, which is placed in mass fraction, is
In 12% sulfuric acid solution, 3h is boiled, it is clean wash with distilled water after taking-up；
Coating sintering step：The titanium-base uniformly mixed noble coatings solution being coated in after pickling etching process
On, it coats, dry, sintering processes repeatedly, the number of occurrence is 30 times；Drying temperature is 180 DEG C, drying time 20min；Sintering
Temperature is 480 DEG C, sintering time 20min；
The more flat step of high temperature：The Ti electrode that coating sintering is completed is subjected to the relatively flat processing of high temperature in fixture, high temperature is relatively flat
Temperature is 480 DEG C, soaking time 3h, and guarantee titanium-based plate flatness is 0.2mm.
Comparative example 1
A kind of technology for preparing electrode, including：
Cutting step：It is the titanium plate of 2.0mm as titanium-base to select thickness, using line cutting technology by titanium-base according to figure
Paper cutting processing；
High-temperature annealing step：Titanium-base after routinely blasting craft sandblasting is carried out to the relatively flat place of high annealing in fixture
Reason, high temperature anneal temperature are 1000 DEG C, soaking time 2.0h, and guarantee titanium-based plate flatness is 0.15mm；
Alkali cleaning deoiling step：Titanium-base is carried out at alkali cleaning oil removing, titanium-base is placed in the hydroxide that mass fraction is 8%
In sodium solution, temperature is constant, and at 90 DEG C, power is 2000W ultrasonic activation 30min, clean wash with distilled water after taking-up；
Pickling etching step：Titanium-base is subjected to pickling etching process, the titanium-base after alkali cleaning, which is placed in mass fraction, is
In 12% sulfuric acid solution, 3h is boiled, it is clean wash with distilled water after taking-up；
Coating sintering step：By uniformly mixed noble coatings solution coated on treated titanium-base, apply repeatedly
It covers, dry, sintering processes, the number of occurrence is 30 times；Drying temperature is 180 DEG C, drying time 20min；Sintering temperature is 480
DEG C, sintering time 20min；
The more flat step of high temperature：The Ti electrode that coating sintering is completed is subjected to the relatively flat processing of high temperature in fixture, high temperature is relatively flat
Temperature is 480 DEG C, soaking time 3h, and guarantee titanium-based plate flatness is 0.2mm.
Effect assessment and performance detection
Distinguish the Ti electrode acquired in Example 1-3 and comparative example 1, carry out correlated performance test, test method is
Traditional test methods, test result is as follows shown in table 1.
The performance test results record sheet of table 1 embodiment 1-3 and 1 Ti electrode of comparative example
It can be obtained from the record in table 1, the electrode of the technology for preparing electrode that the embodiment of the present invention is provided, the acquisition has
Increase with coating binding force, the specific surface area increase of electrode, electric conductivity enhance, chlorine evolution potential reduces, the reinforcing life time is grown etc.
Advantage, to realize that electrolytic efficiency raising in electrolytic process, electrolytic cell calorific value reduction, operation energy consumption reduces, electrode uses the longevity
The advantages such as life length.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (10)
1. a kind of technology for preparing electrode with long service life, which is characterized in that including sandblasting polishing step：Electrode matrix is taken, it will
The electrode matrix is placed in sand-blasting machine, and setting blasting pressure is 0.5-1MPa, and sandblasting angle is 45-90 °, and sand grains flow is 5-
The roughness of 10Kg/h, blast time 2-6min, coordination electrode matrix are 4-10 μm.
2. technology for preparing electrode with long service life as described in claim 1, which is characterized in that sand grains type be corundum,
One kind in silicon carbide sand and aluminum oxide sand or arbitrary combination.
3. technology for preparing electrode with long service life as described in claim 1, which is characterized in that the granularity of sand grains is 30-75
Mesh.
4. technology for preparing electrode with long service life as described in claim 1, which is characterized in that further include cutting step：It takes
The electrode base material is cut into preset shape, obtains electrode matrix, then spray the electrode matrix of acquisition by electrode base material
Sand is polished；
Alkali cleaning deoiling step：The electrode matrix is placed in aqueous slkali after sandblasting is polished and carries out ultrasonic activation, then take
Go out and is cleaned up with clear water；
Pickling etching step：The electrode matrix is placed in acid solution and heats and boil after alkali cleaning oil removing, then takes out simultaneously
It is cleaned up with clear water；
Coating sintering step：Noble metal-coating coating solution, drying is repeated after overpickling etches in the electrode matrix successively
And sintering processes.
5. technology for preparing electrode with long service life as claimed in claim 4, which is characterized in that in the cutting step,
The electrode base material is the metallic plate that thickness is 1-2mm, is cut the electrode base material using wire cutting or laser cutting method
At preset shape；
In the coating sintering step, the number that coating, drying and sintering processes are repeated is 20-30 times；Drying temperature
It is 110-180 DEG C, drying time 10-20min；Sintering temperature is 420-480 DEG C, sintering time 10-20min.
6. technology for preparing electrode with long service life as claimed in claim 4, which is characterized in that in the alkali cleaning deoiling step
In, the electrode matrix after sandblasting is polished, be placed in mass fraction be 6-12% sodium hydroxide solution in, temperature it is constant
70-90 DEG C, power is clean wash with distilled water after taking-up to vibrate 20-40min in the ultrasonic wave of 1000-2000W；
In the pickling etching step, the electrode matrix is placed in the sulphur that mass fraction is 5-12% after alkali cleaning oil removing
In acid solution, 1-3h is boiled, it is clean wash with distilled water after taking-up.
7. technology for preparing electrode with long service life as claimed in claim 4, which is characterized in that further include high annealing step
Suddenly：The electrode matrix carries out high annealing after sandblasting is polished, and the temperature of high annealing is 600-1000 DEG C, when heat preservation
Between be 1-3h, the flatness of coordination electrode matrix is 0.1-0.15mm.
8. technology for preparing electrode with long service life as claimed in claim 4, which is characterized in that further include the relatively flat step of high temperature
Suddenly：The electrode matrix carries out high temperature and relatively puts down after coating sintering, and the more flat temperature of high temperature is 420-480 DEG C, soaking time
Flatness for 1-3h, coordination electrode matrix is 0.1-0.2mm.
9. technology for preparing electrode with long service life as described in claim 1, which is characterized in that the sand-blasting machine is suction-type
Dry blasting machine.
10. such as claim 1-9 any one of them technology for preparing electrode with long service life, which is characterized in that the electrode
Matrix is Titanium base.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110690459A (en) * | 2019-09-25 | 2020-01-14 | 中国华能集团清洁能源技术研究院有限公司 | Method for improving catalytic performance of electrode of molten carbonate fuel cell |
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