CN116511208A - Recycling treatment method of waste catalytic ceramic fiber filter tube - Google Patents
Recycling treatment method of waste catalytic ceramic fiber filter tube Download PDFInfo
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- CN116511208A CN116511208A CN202310445424.8A CN202310445424A CN116511208A CN 116511208 A CN116511208 A CN 116511208A CN 202310445424 A CN202310445424 A CN 202310445424A CN 116511208 A CN116511208 A CN 116511208A
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 89
- 239000000919 ceramic Substances 0.000 title claims abstract description 70
- 239000000835 fiber Substances 0.000 title claims abstract description 68
- 239000002699 waste material Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000004064 recycling Methods 0.000 title claims abstract description 33
- 238000004140 cleaning Methods 0.000 claims abstract description 53
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 238000000576 coating method Methods 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000011069 regeneration method Methods 0.000 claims abstract description 13
- 239000013543 active substance Substances 0.000 claims abstract description 12
- 230000008929 regeneration Effects 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000002585 base Substances 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 16
- 239000011149 active material Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- 230000005587 bubbling Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 7
- 239000002910 solid waste Substances 0.000 abstract description 3
- 229910000510 noble metal Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 28
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910052720 vanadium Inorganic materials 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 8
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000003365 glass fiber Substances 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 238000000605 extraction Methods 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- 239000000428 dust Substances 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000007667 floating Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 238000010200 validation analysis Methods 0.000 description 2
- 150000003681 vanadium Chemical class 0.000 description 2
- WJYAJBDKANFOID-UHFFFAOYSA-N 2-(dodecylamino)propanoic acid Chemical compound CCCCCCCCCCCCNC(C)C(O)=O WJYAJBDKANFOID-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- -1 hg and the like) Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
- B09B3/35—Shredding, crushing or cutting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B2101/00—Type of solid waste
- B09B2101/60—Ceramics, e.g. pottery
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention provides a recycling treatment method of waste catalytic ceramic fiber filter tubes, which is divided into a first type filter tube with a perfect base layer and a second type filter tube with a severe base layer damage according to the damage and fracture degree of waste catalytic ceramic fibers, and the waste catalytic ceramic fiber filter tubes are classified. The method comprises the steps of carrying out regeneration treatment on a first type filter tube, wherein the regeneration treatment comprises at least one catalyst coating liquid coating and drying calcination treatment on the first type filter tube until the content of catalytic active substances in the first type filter tube is recovered to an effective catalytic content; and (3) recycling the second type filter tube, namely cleaning and dissolving the second type filter tube, and recycling the cleaned and dissolved solids and cleaning liquid through solid-liquid separation. The method realizes the classification treatment of the waste catalytic ceramic fiber filter tubes, improves the recovery rate of the waste catalytic ceramic fiber filter tubes and noble metals, and reduces the secondary pollution of solid wastes.
Description
Technical Field
The invention relates to the technical field of catalyst recovery and regeneration, in particular to a recycling treatment method of a waste catalytic ceramic fiber filter tube.
Background
Catalytic ceramic fiber filter tube can simultaneously control dust SO x 、NO x And VOCs and other atmospheric pollutants can greatly reduce the occupation area and construction investment of environmental protection facilities, effectively reduce the running cost, and can become one of the mainstream technical routes of future environmental protection treatment.
However, in addition to a large amount of dust and gas pollutants, the conventional tail gas contains a part of harmful components such as heavy metals (such as Cr, hg and the like), alkaline earth metals (such as Na, K, ca and the like) and ammonium bisulfate, and the like, and in the use process of the catalytic ceramic fiber filter tube, the continuous enrichment of the harmful components thoroughly fails, so that the filter tube is replaced, the cost is high, and the filter tube adsorbing the harmful components also causes secondary pollution. In order to avoid resource waste in the replacement process of the ceramic filter tube, a regeneration mode is adopted for part of the catalytic ceramic fiber filter tube with qualified mechanical strength in the prior art, such as a regeneration method and regeneration equipment for the deactivated catalytic ceramic filter tube disclosed in Chinese patent publication numbers CN112090453A and CN 115007223A, the deactivated catalytic ceramic fiber filter tube is subjected to ash removal, cleaning, drying, spraying catalyst active liquid again, drying, roasting and packaging, and the regenerated catalytic ceramic fiber filter tube is reapplied to production.
However, the above scheme still has the problems of resource waste, environmental pollution and the like caused by the fact that the waste ceramic fiber filter tube which cannot be regenerated cannot be completely recovered.
Disclosure of Invention
In order to overcome the defects in the prior art, the first aspect of the invention provides a recycling treatment method of a waste catalytic ceramic fiber filter tube, which specifically comprises the following steps: classifying the waste ceramic fiber filter tubes into a first type filter tube with a good base layer and a second type filter tube with a broken base layer according to the base layer integrity of the waste catalytic ceramic fiber filter tubes; the method comprises the steps of carrying out regeneration treatment on a first type of filter tube, and specifically comprises the steps of carrying out at least one-time coating and drying calcination treatment on the first type of filter tube by using a catalyst coating liquid until the content of catalytic active substances in the first type of filter tube is recovered to a specified content; and (3) recycling the second-class filter tube, wherein the method specifically comprises the steps of cleaning and dissolving the second-class filter tube, and recycling the cleaned and dissolved solids and cleaning liquid through solid-liquid separation.
Further, the first type filter tube is subjected to catalytic active material detection to obtain the residual quantity of the catalytic active material of the base layer, and the content of the catalytic active material in the catalyst coating liquid is determined according to the residual quantity of the catalytic active material of the base layer.
Further, the first type of filter tube is subjected to classified cleaning and then is subjected to active material detection, and the classified cleaning sequentially comprises ultrasonic cleaning, spray cleaning, primary bubbling cleaning and secondary bubbling cleaning.
Further, the cleaning liquid adopted for the graded cleaning of the first type filter tube is surfactant solution, alkaline solution, acid cleaning solution and clear water in sequence.
Further, the second type filter tube is cleaned and dissolved by adopting a strong alkali solution with the pH value more than 11.
Further, the solids obtained by the recovery treatment of the second type of filter tube are sequentially subjected to heat treatment and superfine grinding, wherein the superfine grinding specifically comprises grinding the heat-treated solids into solid particles with the particle size of 2-10 mu m.
Further, the solids in the second type of filter tube comprise glass fibers and TiO 2 The superfine ground solid is used for glass fiber generation again as a production additive. Wherein, a small amount of heavy metal toxic substances are vitrified and sealed after being melted at high temperature in the subsequent production of glass fiber again, thereby reducing environmental pollution.
Further, the catalytically active material dissolved in the second type filter tube is V 2 O 5 The recovery treatment also comprises the extraction of vanadium in the filtrate after solid-liquid separation.
Further, the drying and calcining treatment of the first type filter tube comprises drying at 120-150 ℃ and calcining at 430-450 ℃ respectively, wherein the heating rate is 10 ℃/min.
Further, the second type filter tube is subjected to heat treatment, namely, the temperature is increased to 750 ℃ at 20 ℃/min, and the volatile components and the moisture are removed by calcining.
According to the invention, the catalytic ceramic fiber filter tubes are divided into the first type filter tubes with the intact base layers and the second type filter tubes with the severely damaged base layers according to the damage and fracture degrees of the base layers, so that the classification treatment of the waste catalytic ceramic fiber filter tubes is realized, the recovery of the waste catalytic ceramic fiber filter tubes is effectively improved, the secondary solid waste pollution is avoided, the performances of the regenerated catalytic ceramic fiber filter tubes are ensured, and the recycling value of the regenerated catalytic ceramic fiber filter tubes is improved.
Drawings
The accompanying drawings illustrate embodiments and, together with the description, serve to explain the principles of the present application. The elements of the drawings are not necessarily to scale relative to each other. Like reference numerals designate corresponding similar parts.
FIG. 1 is a schematic flow chart of a recycling treatment of waste catalytic ceramic fiber filter tubes in an embodiment of the invention.
Detailed Description
The following describes examples of the present application to better understand the present application, and many of the intended advantages of other embodiments and embodiments can be appreciated from the detailed description that follows. It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising" does not exclude the presence of additional identical elements in a process, method, article, or apparatus that comprises an element. Components of embodiments may be positioned in a number of different orientations, and so directional terminology, such as "top," "bottom," "left," "right," "up," "down," etc., is used with reference to the orientation of the figures to describe some embodiments. It is to be understood that the directional terminology is used for purposes of illustration and not limitation.
Fig. 1 is a schematic flow chart of a recycling treatment of a waste catalytic ceramic fiber filter tube in an embodiment of the application. The recycling treatment method of the waste catalytic ceramic fiber filter tube of the embodiment carries out classification treatment based on the integrity degree of the base layer of the waste catalytic ceramic fiber filter tube, and can regenerate the filter tube with the intact base layer by recoating the catalyst, and can not regenerate the filter tube with the severely damaged base layer. Before the integrity of the base layer of the waste catalytic ceramic fiber filter tube is checked, the waste catalytic ceramic fiber filter tube is subjected to pretreatment, specifically, the waste catalytic ceramic fiber filter tube is subjected to ash removal and polishing, the floating ash on the surface of the filter tube is purged by oil removal and water removal pressure water and air, and the deep layer deposited ash on the surface layer and the inside of the filter tube is ground by polishing equipment. The polishing time is determined according to the dust accumulation depth, and the polishing depth is 3-5mm on the surface of the base layer. Checking the integrity of the base layer of the waste catalytic ceramic fiber filter tube after the ash removal and polishing are finished, and classifying the waste catalytic ceramic fiber filter tube into a first type filter tube with a qualified base layer being intact and a second type filter tube with a disqualified base layer being damaged; the second type of filter tube with broken base layer refers to a filter tube with severely broken base layer, which can not be regenerated to recover the catalytic activity.
And (3) carrying out regeneration treatment on the first type filter tube, wherein the regeneration treatment comprises at least one catalyst coating liquid coating and drying and calcining treatment on the first type filter tube until the content of the catalytic active substances in the first type filter tube is recovered to the effective catalytic content. The cleaning is classified cleaning, and ultrasonic cleaning, spray cleaning, primary bubbling cleaning and secondary bubbling cleaning are sequentially carried out in low-concentration surfactant solution, extremely low-concentration alkaline solution, low-concentration acidic solution and clear water. Detecting the content of the catalytic active substances in the cleaned first-class filter tubes, designing a catalyst coating liquid according to the content of the catalytic active substances, and coating the catalyst coating liquid on the first-class filter tubes on corresponding equipment. The coating can be performed by dipping coating, forward pressurizing coating, reverse negative pressure coating or the like. And carrying out heat treatment on the coated first-type filter tube, wherein the heat treatment is drying and calcining, and then detecting the active substances in the first-type filter tube. And (3) determining the effective catalytic content of the catalytic active substances of the filter tubes according to the actual conditions, re-applying the filter tubes to engineering if the content is detected to be qualified, and re-applying the filter tubes if the content is detected to be unqualified until the content of the catalytic active substances of the first type of filter tubes reaches the standard, so that the catalytic activity of the filter tubes is recovered.
And (3) recycling the second-class filter tube, namely cleaning and dissolving the second-class filter tube, and recycling the cleaned and dissolved solids through solid-liquid separation. According to the research of the inventor, the solid obtained by cleaning, dissolving and solid-liquid separating the second type filter tube comprises glass fiber and TiO 2 The solid particles obtained after superfine grinding treatment can be used for glass fiber generation again as production additives, and in the production of glass fibers again, a small amount of heavy metal toxic substances can be vitrified and sealed after being melted at high temperature (above 1200 ℃), so that environmental pollution is avoided. Specifically, a strong alkali solution with the pH value more than 11 is adopted to clean and dissolve the second type of filter tube, and solid and cleaning liquid are obtained through solid-liquid separation. Heat treating the solid obtained after solid-liquid separation to remove the solidAnd (3) carrying out superfine grinding to obtain solid particles with the particle size of 2-10 mu m, detecting the content of active substances, and directly putting the solid particles into a catalytic ceramic fiber filter tube for re-production.
In one embodiment, the catalytically active material in the spent catalytic ceramic fiber filter tube is V 2 O 5 The recovery treatment also comprises the extraction of vanadium in the filtrate after solid-liquid separation. Specifically, V in the catalyst in the filter tube is washed out by a strong alkali solution 2 O 5 And extracting vanadium-containing substances in the cleaning liquid by adopting an acid method by adopting one or more of organic acid or inorganic acid.
According to the regeneration method of the waste catalytic ceramic fiber filter tube, the catalytic ceramic fiber filter tube is classified according to the damage degree of the waste catalytic ceramic fiber filter tube, so that the recovery efficiency and the recycling value can be improved.
[ example 1 ] 5% V loading 2 O 5 Regeneration of catalytic ceramic fiber filter tubes
Referring to fig. 1, the process of recycling the waste catalytic ceramic fiber filter tube in this embodiment is as follows:
1. purging the waste catalytic ceramic fiber filter tube with oil removal and water removal compressed air to remove floating ash, and grinding the accumulated ash and the base layer which are positioned on the surface layer and the inside of the filter tube by about 5mm through grinding equipment;
2. and screening to obtain qualified first-class filter tubes with the intact base layers and unqualified second-class filter tubes with the severely damaged base layers through checking the intact base layers of the waste catalytic ceramic fiber filter tubes, and carrying out classification treatment.
3. And cleaning the first type of filter tubes, wherein the cleaning is classified cleaning. Ultrasonic cleaning is carried out for 2 hours in a mixed solution of lauric acid and dodecylaminopropionic acid with the weight percentage of 0.3 percent, then spray cleaning is carried out for 20 minutes in a KOH solution with the weight percentage of 0.001M, bubbling cleaning is carried out for 1 hour in an oxalic acid solution with the weight percentage of 0.001M, and finally bubbling cleaning is carried out for 3 hours by using clean water. Through active material detection, the catalytic active material V in the waste catalytic ceramic fiber filter tube is confirmed 2 O 5 The residual amount is about 2%.
4. Inspection according to step 3Measurement results, determine the content of V in the catalyst coating liquid formula 2 O 5 The content was 3.5%, and then the catalyst coating liquid was loaded onto the cleaned first type filter tube by dip coating.
5. Carrying out heat treatment on the coated first type filter tube, and drying at 120 ℃ and calcining at 450 ℃ at a heating rate of 10 ℃/min; validation of V in filter tube by detection 2 O 5 After the content is more than 5%, the method is reapplied to engineering; if the V in the catalytic ceramic fiber filter tube does not reach the standard, the V in the catalytic ceramic fiber filter tube 2 O 5 The catalyst coating liquid is redesigned in content, and the secondary coating is performed.
6. And (3) directly cleaning and dissolving the unqualified second type filter tube by using KOH solution with pH of 11, and carrying out solid-liquid separation by using equipment to obtain solid and cleaning liquid.
7. Oxalic acid and sulfamic acid are added into the cleaning liquid, and free vanadium in the cleaning liquid is converted into vanadium-containing substances such as vanadium salt and the like for extraction.
8. The solid is subjected to heat treatment, and is directly heated to 750 ℃ at a heating rate of 20 ℃/min for drying and calcining, so that moisture and organic matters are thoroughly removed.
9. Grinding the dried and calcined solid into small particles with the particle diameter less than 5 μm after superfine grinding, and detecting V 2 O 5 The content is directly used for the production of ceramic fiber filter tubes.
[ example 2 ] 7% V loading 2 O 5 Regeneration of catalytic ceramic fiber filter tubes
Example 1 differs from example 2 in that in this example the raw V of the regenerated catalytic ceramic fiber filter tube 2 O 5 The loading was 7%; the polishing depth of the surface of the base layer is 4mm; the step cleaning sequentially adopts 0.5wt.% of mixed solution of lauric acid-quaternary ammonium salt-dodecylaminopropionic acid, 0.001M NaOH solution, 0.0005M nitric acid and carboxyacetic acid solution and clear water; the first type of filter tube heat treatment comprises drying at 150 ℃ and calcining at 430 ℃, wherein the heating rate is 10 ℃/min; cleaning and dissolving NaOH solution with pH of 12 for the second type filter tube; oxalic acid and citric acid are adopted to extract vanadium.
Reference is made to the drawings1, in this example, 7% V is supported 2 O 5 The waste catalytic ceramic fiber filter tube recycling treatment process comprises the following steps:
1. purging the waste catalytic ceramic fiber filter tube with oil removal and water removal compressed air to remove floating ash, and grinding the accumulated ash and the base layer which are positioned on the surface layer and the inside of the filter tube by about 4mm through grinding equipment;
2. and screening to obtain qualified first-class filter tubes with the intact base layers and unqualified second-class filter tubes with the severely damaged base layers through checking the intact base layers of the waste catalytic ceramic fiber filter tubes, and carrying out classification treatment.
3. And cleaning the first type of filter tubes, wherein the cleaning is classified cleaning. Ultrasonic cleaning in 0.5wt.% lauric acid-quaternary ammonium salt-dodecylaminopropionic acid mixed solution for 2h, spray cleaning in 0.001M NaOH solution for 30min, bubbling cleaning in 0.0005M nitric acid and carboxyacetic acid solution for 2h, bubbling cleaning with clear water for 4h, and detecting and confirming V in the filter tube by active substance 2 O 5 The residual amount was about 3.5%.
4. According to the detection result of the step 3, determining that the catalyst coating liquid contains V 2 O 5 The content was 3.5%, and then the catalyst coating liquid was loaded onto the cleaned first type filter tube by a forward pressurized coating method.
5. Carrying out heat treatment on the coated first type filter tube, drying at 150 ℃ and calcining at 430 ℃, wherein the heating rate is 10 ℃/min; validation of V in filter tube by detection 2 O 5 After the content is more than 7%, the method is reapplied to engineering; if the V in the catalytic ceramic fiber filter tube does not reach the standard, the V in the catalytic ceramic fiber filter tube 2 O 5 The catalyst coating liquid is redesigned in content, and the secondary coating is performed.
6. And (3) directly cleaning and dissolving the unqualified second type of filter tube by using NaOH solution with the pH value of 12, and carrying out solid-liquid separation by using equipment to obtain solid and cleaning liquid.
7. Oxalic acid and citric acid are added into the cleaning solution, and free vanadium in the cleaning solution is converted into vanadium-containing substances such as vanadium salt and the like for extraction.
8. The solid is subjected to heat treatment, and is directly heated to 750 ℃ at a heating rate of 20 ℃/min for drying and calcining, so that moisture and organic matters are thoroughly removed.
9. Grinding the dried and calcined solid into small particles with the particle diameter less than 5 μm after superfine grinding, and detecting V 2 O 5 The content is directly used for the production of ceramic fiber filter tubes.
Examples 1-2 above disclose the recycling treatment method of waste catalytic ceramic fiber filter tubes according to the present invention for V-containing 2 O 5 According to the scheme, the waste catalytic ceramic fiber filter tubes are effectively screened and classified, secondary solid waste pollution is avoided, various performances of the regenerated catalytic ceramic fiber filter tubes are guaranteed, and the recycling value of the regenerated catalytic ceramic fiber filter tubes is improved.
The foregoing is a preferred embodiment of the present application, and it will be apparent to those skilled in the art that various modifications and variations can be made to the embodiment of the present application without departing from the spirit and scope of the application. In this manner, the present application is also intended to cover such modifications and changes as fall within the scope of the claims of the application and the equivalents thereof.
Claims (9)
1. A recycling treatment method of a waste catalytic ceramic fiber filter tube is characterized by comprising the following steps:
classifying the waste catalytic ceramic fiber filter tubes into a first type filter tube with a good base layer and a second type filter tube with a broken base layer according to the integrity degree of the base layer of the waste catalytic ceramic fiber filter tubes;
the first type filter tube is subjected to regeneration treatment, and specifically comprises the steps of coating the first type filter tube with a catalyst coating liquid at least once, drying and calcining until the content of the catalytic active substances in the first type filter tube is recovered to an effective catalytic content;
and (3) recycling the second-class filter tube, wherein the method specifically comprises the steps of cleaning and dissolving the second-class filter tube, and recycling the cleaned and dissolved solids and cleaning liquid through solid-liquid separation.
2. The method for recycling waste catalytic ceramic fiber filter tubes according to claim 1, wherein the first type of filter tubes are subjected to catalytic active material detection to obtain the residual amount of the catalytic active material of the base layer, and the content of the catalytic active material in the catalyst coating liquid is determined according to the residual amount of the catalytic active material of the base layer.
3. The method for recycling the waste catalytic ceramic fiber filter tube according to claim 2, further comprising: and performing grading cleaning on the first type of filter pipes, and then performing active material detection, wherein the grading cleaning sequentially comprises ultrasonic cleaning, spray cleaning, primary bubbling cleaning and secondary bubbling cleaning.
4. The recycling treatment method of the waste catalytic ceramic fiber filter tubes according to claim 3, wherein the cleaning liquid adopted for the classified cleaning of the first type of filter tubes is surfactant solution, alkaline solution, acid washing solution and clear water in sequence.
5. The method for recycling waste catalytic ceramic fiber filter tubes according to claim 1, wherein the second type filter tubes are cleaned and dissolved by using a strong alkali solution with a pH value of more than 11.
6. The recycling treatment method of the waste catalytic ceramic fiber filter tube according to claim 1, wherein the solid obtained by recycling treatment of the second type filter tube is sequentially subjected to heat treatment and superfine grinding, wherein the superfine grinding specifically comprises grinding the heat-treated solid into solid particles with the particle size of 2-10 μm.
7. The recycling treatment method of the waste catalytic ceramic fiber filter tube according to claim 1, wherein the catalytic active substance in the waste catalytic ceramic fiber filter tube is V 2 O 5 The recycling process further comprises extracting theVanadium in the filtrate after solid-liquid separation.
8. The method for recycling waste catalytic ceramic fiber filter tubes according to claim 1, wherein the drying and calcining treatment of the first type of filter tubes comprises drying at 120-150 ℃ and calcining at 430-450 ℃ respectively, and the heating rate is 10 ℃/min.
9. The method for recycling the waste catalytic ceramic fiber filter tube according to claim 6, which is characterized in that,
the second type of filter tube is heat treated by heating to 750 ℃ at 20 ℃/min for calcination to remove volatile components and moisture.
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CN202310445424.8A CN116511208A (en) | 2023-04-24 | 2023-04-24 | Recycling treatment method of waste catalytic ceramic fiber filter tube |
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