CN114405554A - Process for preparing neutral spherical ozone catalyst from red mud - Google Patents
Process for preparing neutral spherical ozone catalyst from red mud Download PDFInfo
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- CN114405554A CN114405554A CN202210040248.5A CN202210040248A CN114405554A CN 114405554 A CN114405554 A CN 114405554A CN 202210040248 A CN202210040248 A CN 202210040248A CN 114405554 A CN114405554 A CN 114405554A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 230000007935 neutral effect Effects 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 23
- 230000003197 catalytic effect Effects 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000004568 cement Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000012798 spherical particle Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000000919 ceramic Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 21
- 239000011148 porous material Substances 0.000 abstract description 14
- 238000005554 pickling Methods 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 4
- 150000001340 alkali metals Chemical class 0.000 abstract description 4
- 230000000593 degrading effect Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 230000003750 conditioning effect Effects 0.000 abstract description 3
- 230000005764 inhibitory process Effects 0.000 abstract description 3
- 238000002468 ceramisation Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a process for preparing a neutral spherical ozone catalyst from red mud, which specifically comprises the following steps: s1, carrying out high-temperature heat treatment on the red mud; s2, preparing red mud powder; s3, acid adjusting the red mud powder; s4, preparing a neutral spherical ozone catalyst; firstly carrying out high-temperature heat treatment on the red mud, then carrying out acid conditioning on the red mud after the high-temperature heat treatment, and adding 0.6kgH into each ton of red mud2SO4Acid conditioning of red mud, pickling and high temperature heat treatmentThe red mud is modified by the process, so that the denitration activity of the red mud catalyst in a medium-high temperature section is greatly improved, the pickling treatment has a good dealkalization effect, the inhibition effect of alkali metal on the catalyst activity is weakened, the pore structure on the surface of the red mud is dredged, the inter-pore connectivity is enhanced, the particle size is refined, the pore volume and the specific surface area are increased, the catalytic oxidation reaction in water treatment is facilitated, and the effect of catalytically degrading pollutants in wastewater is good.
Description
Technical Field
The invention belongs to the technical field of environmental management, and particularly relates to a process for preparing a neutral spherical ozone catalyst from red mud.
Background
Red mud, also known as red mud, is solid waste residue discharged during the production of alumina in the aluminum production industry, and can seriously damage the ecological environment. Every 1t of alumina is produced, 0.7-2.0 t of red mud can be discharged due to different production technology levels and bauxite tastes, the red mud stacking amount and the red mud storage amount are continuously increased along with the continuous improvement of the production level, the red mud disposal mode still mainly adopts open stacking and open dam construction, and a large amount of precious land resources are occupied. Red mud contains radioactive elements and can bring potential safety hazards to air, water, soil and buildings. The environmental pollution caused by the red mud is increasingly serious, so the high-efficiency resource utilization of the red mud is more urgent. The red mud has the advantages of small particle size, low porosity, stable chemical components in water, high specific surface area and the like, and is an excellent low-cost adsorbent. Therefore, the red mud has wide application prospect in wastewater treatment.
The original adsorption capacity of red mud is limited, and the red mud can not be directly used for treating wastewater containing heavy metal ions. In order to prepare a catalyst with excellent performance for catalyzing and degrading pollutants in wastewater, the catalyst is modified by adopting modes of acid activation, heat treatment and the like. The specific surface area of the red mud modified by the prior art is obviously increased, but the effect on catalytic degradation of pollutants in wastewater is to be improved.
Disclosure of Invention
The invention aims to provide a process for preparing a neutral spherical ozone catalyst by using red mud, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a process for preparing a neutral spherical ozone catalyst from red mud specifically comprises the following steps:
s1, high-temperature heat treatment of red mud: putting the red mud into a rotary oven, firstly heating the temperature of the rotary oven to 105 ℃, keeping the temperature constant for 1 hour, then heating the temperature of the rotary oven to 250 ℃, keeping the temperature constant for 2 hours, then adjusting the temperature of the rotary oven to 400-800 ℃, drying the red mud in the rotary oven at 400-800 ℃ for 1.5-2 hours, and carrying out high-temperature heat treatment on the red mud to improve the catalytic performance of the red mud, wherein the red mud is reduced at high temperature, and Fe20s is converted into Fe30 d;
s2, preparing red mud powder: naturally cooling the red mud subjected to high-temperature heat treatment in the step S1 to room temperature, and grinding and sieving the red mud subjected to heat treatment to prepare 300-mesh red mud powder;
s3, acid-regulated red mud powder: adding an acid solution to the red mud powder in the step S2, and adjusting the pH value of the red mud powder to 7;
s4, preparing a neutral spherical ozone catalyst: and (5) adding 25% of adhesive into the mud powder with the acid and the alkali adjusted in the step (S3) to prepare spherical particles with the particle size of 6mm, and naturally drying to obtain the neutral spherical ozone catalyst.
Preferably, the specific surface area of the red mud catalyst in the step S1 is about: 22.8m2And g, in the step S1, the drying temperature of the red mud in the rotary oven is preferably 500 ℃, the red mud is dried at 500 ℃, the red mud is coated with powder, the surface cannot be too smooth, the ceramization is avoided, the material has a large specific surface area and a good pore structure due to the calcination at 500 ℃, and the denitration activity of the catalyst at a high-temperature section is ensured.
Preferably, the acid solution in step S3 is one of nitric acid, hydrochloric acid, sulfuric acid and oxalic acid, preferably sulfuric acid, wherein 0.6kgH is added per ton of red mud2SO4To remove NO3 -、Cr-、SO4 2-、C204 2-、HC204 -And plasma impurity ions.
Preferably, the binder in step S4 is 325 mesh cement silicate.
The invention has the technical effects and advantages that: the process for preparing the neutral spherical ozone catalyst from the red mud comprises the steps of carrying out high-temperature heat treatment on the red mud, then carrying out acid conditioning on the red mud subjected to the high-temperature heat treatment, and adding 0.6kgH into each ton of the red mud2SO4The red mud is subjected to acid adjustment, and is modified by the acid pickling and high-temperature heat treatment process, so that the denitration activity of the red mud catalyst in a medium-high temperature section is greatly improved, the acid pickling treatment has a good dealkalization effect, the inhibition effect of alkali metal on the catalyst activity is weakened, the pore structure on the surface of the red mud is dredged, the inter-pore connectivity is enhanced, the particle size is refined, the pore volume and the specific surface area are increased, the catalytic oxidation reaction in water treatment is facilitated, and the effect of catalytically degrading pollutants in wastewater is good.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a process for preparing a neutral spherical ozone catalyst from red mud as shown in figure 1, which specifically comprises the following steps:
s1, high-temperature heat treatment of red mud: putting the red mud into a rotary oven, firstly heating the temperature of the rotary oven to 105 ℃, keeping the temperature constant for 1 hour, then heating the temperature of the rotary oven to 250 ℃, keeping the temperature constant for 2 hours, then adjusting the temperature of the rotary oven to 400-800 ℃, drying the red mud in the rotary oven at 400-800 ℃ for 1.5-2 hours, and carrying out high-temperature heat treatment on the red mud to improve the catalytic performance of the red mud, wherein the red mud is reduced at high temperature, and Fe20s is converted into Fe30 d;
s2, preparing red mud powder: naturally cooling the red mud subjected to high-temperature heat treatment in the step S1 to room temperature, and grinding and sieving the red mud subjected to heat treatment to prepare 300-mesh red mud powder;
s3, acid-regulated red mud powder: adding an acid solution to the red mud powder in the step S2, and adjusting the pH value of the red mud powder to 7;
s4, preparing a neutral spherical ozone catalyst: and (5) adding 25% of adhesive into the mud powder with the acid and the alkali adjusted in the step (S3) to prepare spherical particles with the particle size of 6mm, and naturally drying to obtain the neutral spherical ozone catalyst.
Preferably, the specific surface area of the red mud catalyst in the step S1 is about: 22.8m2The drying temperature of the red mud in the step S1 in the rotary oven is preferably 500 ℃, the red mud is dried at 500 ℃, the red mud is coated with powder, the surface of the red mud cannot be too smooth, ceramization is avoided, the material has a large specific surface area and a good pore structure due to the calcination at 500 ℃, the denitration activity of the catalyst in a high-temperature section is ensured, the control of the temperature of the red mud is critical, the coating of the red mud at 500 ℃ cannot be too smooth, the ceramization is avoided, the catalytic performance of the red mud is improved after the high-temperature heat treatment, the red mud is reduced at high temperature, and Fe20S is converted into Fe30 d.
The acid solution in the step S3 is one of nitric acid, hydrochloric acid, sulfuric acid and oxalic acid, preferably sulfuric acid, wherein 0.6kgH is added to each ton of red mud2SO4To remove NO3 -、Cr-、SO4 2-、C204 2-、HC204 -The acid washing treatment has good dealkalization effect due to the impurity ions, weakens the inhibiting effect of alkali metal on the activity of the catalyst, simultaneously dredges the pore structure on the surface of the red mud, enhances the connectivity among pores, refines the particle size, increases the pore volume and the specific surface area and is beneficial to the catalytic oxidation reaction in the water treatment.
The binder in step S4 is 325 mesh cement silicate.
The process for preparing the neutral spherical ozone catalyst by the red mud comprises the steps of carrying out high-temperature heat treatment on the red mud, then carrying out acid adjustment on the red mud after the high-temperature heat treatment,adding 0.6kgH into each ton of red mud2SO4The red mud is subjected to acid adjustment, and is modified by the acid pickling and high-temperature heat treatment process, so that the denitration activity of the red mud catalyst in a medium-high temperature section is greatly improved, the acid pickling treatment has a good dealkalization effect, the inhibition effect of alkali metal on the catalyst activity is weakened, the pore structure on the surface of the red mud is dredged, the inter-pore connectivity is enhanced, the particle size is refined, the pore volume and the specific surface area are increased, the catalytic oxidation reaction in water treatment is facilitated, and the effect of catalytically degrading pollutants in wastewater is good.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (4)
1. A process for preparing a neutral spherical ozone catalyst from red mud is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, high-temperature heat treatment of red mud: putting the red mud into a rotary oven, firstly heating the temperature of the rotary oven to 105 ℃, keeping the temperature constant for 1 hour, then heating the temperature of the rotary oven to 250 ℃, keeping the temperature constant for 2 hours, then adjusting the temperature of the rotary oven to 400-800 ℃, drying the red mud in the rotary oven at 400-800 ℃ for 1.5-2 hours, and carrying out high-temperature heat treatment on the red mud to improve the catalytic performance of the red mud, wherein the red mud is reduced at high temperature, and Fe20s is converted into Fe30 d;
s2, preparing red mud powder: naturally cooling the red mud subjected to high-temperature heat treatment in the step S1 to room temperature, and grinding and sieving the red mud subjected to heat treatment to prepare 300-mesh red mud powder;
s3, acid-regulated red mud powder: adding an acid solution to the red mud powder in the step S2, and adjusting the pH value of the red mud powder to 7;
s4, preparing a neutral spherical ozone catalyst: and (5) adding 25% of adhesive into the mud powder with the acid and the alkali adjusted in the step (S3) to prepare spherical particles with the particle size of 6mm, and naturally drying to obtain the neutral spherical ozone catalyst.
2. The process for preparing the neutral spherical ozone catalyst by using the red mud as claimed in claim 1, which is characterized in that: the specific surface area of the red mud catalyst in the step S1 is about: 22.8m2And g, in the step S1, the drying temperature of the red mud in the rotary oven is preferably 500 ℃, the red mud is dried at 500 ℃, the red mud is coated with powder, the surface cannot be too smooth, and the ceramic formation is avoided.
3. The process for preparing the neutral spherical ozone catalyst by using the red mud as claimed in claim 1, which is characterized in that: the acid solution in the step S3 is one of nitric acid, hydrochloric acid, sulfuric acid and oxalic acid, preferably sulfuric acid, wherein 0.6kgH is added to each ton of red mud2SO4。
4. The process for preparing the neutral spherical ozone catalyst by using the red mud as claimed in claim 1, which is characterized in that: the binder in step S4 is 325 mesh cement silicate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210040248.5A CN114405554A (en) | 2022-01-14 | 2022-01-14 | Process for preparing neutral spherical ozone catalyst from red mud |
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| CN202210040248.5A CN114405554A (en) | 2022-01-14 | 2022-01-14 | Process for preparing neutral spherical ozone catalyst from red mud |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115448726A (en) * | 2022-09-05 | 2022-12-09 | 南京工业大学 | Method for enhancing catalytic performance of silicon carbide film material by acid etching |
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| CN105107510A (en) * | 2015-09-10 | 2015-12-02 | 广西大学 | Modified red mud and preparation method and application thereof |
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2022
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| CN102886247A (en) * | 2012-09-29 | 2013-01-23 | 广西大学 | Method for preparing adsorbent by virtue of red mud in alumina industry and sludge in sewage treatment |
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| CN105107510A (en) * | 2015-09-10 | 2015-12-02 | 广西大学 | Modified red mud and preparation method and application thereof |
| KR20170119365A (en) * | 2016-04-18 | 2017-10-27 | 한경대학교 산학협력단 | Adsorbent for fluoride removal by red mud and preparing method thereof |
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Cited By (2)
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| CN115448726B (en) * | 2022-09-05 | 2024-02-06 | 南京工业大学 | Method for enhancing catalytic performance of silicon carbide film material by acid etching |
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