CN1557714A - Method for preparing active aluminum oxide utilizing industrial sludge of aluminium section bar plant - Google Patents
Method for preparing active aluminum oxide utilizing industrial sludge of aluminium section bar plant Download PDFInfo
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- CN1557714A CN1557714A CNA2004100140319A CN200410014031A CN1557714A CN 1557714 A CN1557714 A CN 1557714A CN A2004100140319 A CNA2004100140319 A CN A2004100140319A CN 200410014031 A CN200410014031 A CN 200410014031A CN 1557714 A CN1557714 A CN 1557714A
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- sludge
- activated alumina
- nitric acid
- dilute nitric
- acid solution
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Abstract
The present invention belongs to the field of the comprehensive utilization of waste solid, and is especially to biological environment material technology. The production process of active alumina with industrial sludge from aluminum section factory includes depositing waste liquid to obtain sludge as solid waste with main components of gamma-AlOOH and Al(OH)3 and amorphous structure; and mixing dilute nitric acid with dry sludge to form plastic mud and to obtain active alumina with crystal phase gamma-Al2O3. The prepared active alumina is white or grey sphere, column or other grain, and has great specific surface area and great porosity.
Description
Technical field:
The present invention relates to utilize the method for waste aluminum sludge for the feedstock production activated alumina, belong to the comprehensive utilization of solid waste, exactly, it is the technical field of ecological environment material nd.
Technical background:
Waste aluminum sludge is that the aluminium shape surface treating processes produces a large amount of waste liquids, and it is milky colloidal solution, the ultra-fine and high dispersing of particle.This waste liquid is in case discharge inevitable serious environment pollution and river waters, destruction ecology.Therefore before the discharging of waste liquid, a large amount of mud that treating processes must be produced are removed.Factory adopts precipitation and filter method, filters solid mud, the filtrate discharge of remaining clarification.This solid mud main component is γ-AlOOH, Al (OH)
3With solid matter with amorphous body structure.Sludge moisture content is up to 70-80%, and this amount of sludge is very big, and a large aluminum profile factory can produce 25-30 ton mud every day, the 800-900 ton is arranged, annual recyclable more than 10,000 tons in every month.There are tens families in domestic large aluminum profile enterprise, and there is family more than 100 in medium and small sized enterprises, and annual to produce industrial sludge quantity very big.Have a strong impact on the comprehensive regulation and the ordinary production of aluminium section bar plant waste liquid, seriously cause the secondary pollution of aluminium section bar plant.Therefore the comprehensive utilization of mud is essential, has important environment protection significance.The present invention utilizes waste aluminum sludge to prepare activated alumina, does not need the preparation process through aluminium hydroxide, greatly reduces the production cost of activated alumina, and economic benefit is very remarkable.
By retrieval, Chinese patent publication number 1051541 relate to employing with aluminium section bar processing waste residue directly with the operational path of hydrochloric acid reaction, decolouring by charcoal absorption obtains water white liquid polymeric aluminum oxide; Chinese patent publication number 1350065 relates to the sulfur waste acid that produces with waste Aluminum slag and aluminium shape surface chemical treatment, useless sodium hydroxide is raw material, preparation Tai-Ace S 150, sodium aluminate and aluminium hydroxide; Light reel number: 1993GC14 relates to and utilizes Al (OH)
3Gel waste residue is produced polymer alumina; Light reel number: 2000GC26 relates to the research that utilizes aluminum dross to produce water conditioner one Tai-Ace S 150; Light reel number: 1995GC23 relates to and utilizes the alumilite process aluminum dross to produce Tai-Ace S 150; International online retrieval is not reported for work and is utilized the aluminium section bar industrial sludge to prepare activated alumina.Therefore, do not report for work as yet both at home and abroad and utilize waste aluminum sludge to prepare activated alumina, this project belongs to the technology and the technology of first research invention both at home and abroad.
Summary of the invention:
The objective of the invention is to utilize waste aluminum sludge to prepare the method for activated alumina.
The object of the present invention is achieved like this, and production stage is that the aluminium shape surface processing procedure produces a large amount of waste liquids for (1) this mud, and through the solid slag that sedimentation and filtration obtains, this mud main component is γ-AlOOH, Al (OH)
3With the solid matter with amorphous body structure; (2) adopt nitrate method: in through the dewatered sludge powder that grinds, adding dilute nitric acid solution and certain proportion dewatered sludge mixes and pugging, perhaps directly add water mixing pugging, form the plasticity walk, it is that 4-8mm is spherical that walk be may be formed into particle diameter, 100 ℃ of oven dry, after the drying, 400-900 ℃ of sintering, the sintered heat insulating time is 1-6 hour, obtains with γ-Al
2O
3Activated alumina for crystalline phase; (3) the activated alumina outward appearance of preparation is that white and linen orbicule, column or other are granular, and particle diameter is 3-7mm, its performance: specific area is 180-450m
2/ g, average pore size is 3-7nm, pore volume is 0.15-0.8cm
3/ g, water absorption rate 〉=50%, rupture strength 〉=70N/ ball.
The present invention compared with prior art has following novelty and advantage: 1) raw material and technological innovation: it is main material that prior art adopts commercial alumina, and this project employing waste aluminum sludge is raw material, innovation with raw material and technology, therefore the project that belongs to multipurpose use of solid waste and turn waste into wealth has great environment protection significance.2) the present invention compared with prior art, it is ultra-fine that the industrial sludge that this project adopts has particle, part is crystal, part is amorphous body, surface area is big, active high characteristics are conducive to mud and change into γ-Al
2O
3, its conversion ratio height.3) transformation rule of the present invention is different with prior art transformation rule.Change law of the present invention: mud changes γ-Al at 500-1100 ℃
2O
3, change α-Al at 1100-1200 ℃
2O
3And the prior art change law: from γ-Al
2O
3Or Al (OH)
3Change α-Al into
2O
3Need the transformation through several middle variants, just can change α-Al into
2O
34) the present invention adopts industrial sludge to prepare activated alumina does not need preparation process through aluminium hydroxide, and prior art need to through the preparation process of aluminium hydroxide, therefore reduce the preparation cost of activated alumina greatly.5) compared with prior art raw materials cost is very low in the present invention, and economic benefit and social benefit are very remarkable, have the very strong market competitiveness, so investment risk is little.6) to prepare the activated alumina specific surface area be 180-400m in the present invention
2/ g, and the specific surface area of prior art is 150-300m
2/ g.So it is bigger than prior art that the present invention prepares the activated alumina specific surface area.
Take waste aluminum sludge as raw material, in dewatered sludge, add certain density dilute nitric acid solution, constantly stir pugging, form the plasticity walk.Walk is molded into granular (other shapes) base substrate that diameter is 4-6mm, after the drying, places high temperature furnace 400-900 ℃ calcining, temperature retention time is 1-6 hour, is cooled to then room temperature, and its crystalline phase is γ-Al
2O
3The raw material that the present invention adopts is an industrial sludge, and it is a solid waste, rather than commercial alumina, need be through the preparation process of aluminium hydroxide, so have raw material and technical innovation.
Embodiment:
Aluminium section bar industrial sludge dewatered drying obtains dewatered sludge, its composition: SiO
22-3%, Al
2O
3Be 60-65%, loss on ignition is 33-35%, and other impurity are 0.8-1.2%, with chamotte crushing with grind to form 320 sieve meshes.Add dilute nitric acid solution in the dewatered sludge of having weighed, constantly stir pugging, form the plasticity walk.Dilute nitric acid solution concentration: concentrated nitric acid: H
2O=1: 1-1: 10, dilute nitric acid solution: dewatered sludge=1: 1.1-1: 3.With extrusion moulding and rotation comminution granulation, it is 4-8mm spherolite base substrate that plastic walk is molded into diameter, and oven dry moved into the baking room oven dry after 24 hours naturally.To dry granular particle and pack in the saggar, and place High Temperature Furnaces Heating Apparatus to calcine, sintering temperature is 400-900 ℃, and the sintered heat insulating time is 2 hours, and the control heat-up rate is 80 ℃/hour.Calcining sample is tested specific surface area, mean pore size, pore volume, water-intake rate and ultimate compression strength.Test result: specific surface area (BEF) is 180-450mm
2/ g, mean pore size is 3-7nm, pore volume is 0.15-0.8cm
3/ g, water-intake rate 〉=50%, ultimate compression strength 〉=70N/ ball.
Adopt nitrate method: in through the dewatered sludge powder that grinds, adding dilute nitric acid solution and certain proportion dewatered sludge mixes and pugging, perhaps directly add water mixing pugging, form the plasticity walk, it is that 4-8mm is spherical that walk be may be formed into particle diameter, 100 ℃ of oven dry, after the drying, 400-900 ℃ of sintering, the sintered heat insulating time is 1-6 hour, obtains with γ-Al
2O
3Activated alumina for crystalline phase; The dilute nitric acid solution of its narration, the weight ratio of its red fuming nitric acid (RFNA) and water are 1: 1-1: 10, and the weight ratio of dilute nitric acid solution and dewatered sludge is 1: 1-1: 3.
Embodiment 1:
In the dewatered sludge of having weighed, add dilute nitric acid solution, constantly stir pugging, form the plasticity walk.With rotating comminution granulation, it is 4-6mm spherolite base substrate that plastic walk is molded into diameter, naturally oven dry moved into the baking room oven dry after 24 hours, and controlling moisture content is about 5%, to dry spherical particle packs in the saggar, place High Temperature Furnaces Heating Apparatus to calcine, sintering temperature is 450 ℃, and the sintered heat insulating time is 2 hours, the control heat-up rate is 80 ℃/hour, naturally cools to room temperature then.With incinerating product test specific surface area, mean pore size, pore volume, water-intake rate and ultimate compression strength.Test data is listed in the table 1.
Table 1 embodiment 1: salpeter solution concentration is to the activated alumina Effect on Performance
Experiment sequence number HNO
3: H
2O (weight ratio) specific surface area (m
2/ g)) mean pore size (nm) pore volume (cm
3/ g) thing phase
Sample 11: 2 237 3.51 0.16 γ-Al
2O
3
Sample 21: 3 245 3.41 0.16 γ-Al
2O
3
Sample 31: 4 244 4.32 0.17 γ-Al
2O
3
Sample 41: 5 248 5.24 0.22 γ-Al
2O
3
Sample 51: 6 264 4.68 0.27 γ-Al
2O
3
Sample 61: 7 249 4.88 0.48 γ-Al
2O
3
Sample 71: 8 236 6.29 0.24 γ-Al
2O
3
Embodiment 2:
Embodiment 2 is the sour water ratio fixedly, i.e. HNO
3: H
2O=1: 6, change diluted acid and dewatered sludge ratio, inquire into it to effect of material performance.The preparation method is identical with embodiment 1.
Table 2 embodiment 2 dilute nitric acid solution consumptions and dewatered sludge consumption ratio are to material property influence (HNO
3: H
2O)
Experiment sequence number diluted acid/dewatered sludge specific surface area (m
2/ g) mean pore size (nm) pore volume (cm
3/ g) thing phase
Sample 81: 1.5 260 3.25 0.18 γ-Al
2O
3
Sample 91: 1.8 267 3.52 0.20 γ-Al
2O
3
Sample 10 1: 2.1 267 4.04 0.23 γ-Al
2O
3
Sample 11 1: 2.4 264 4.68 0.27 γ-Al
2O
3
Sample 12 1: 2.7 400 4.33 0.46 γ-Al
2O
3
Embodiment 3:
HNO among the embodiment 3
3: H
2O=1: 7, dilute nitric acid solution consumption and dewatered sludge consumption ratio are 1: 2.4, inquire into sintering temperature to effect of material performance.The preparation method is identical with embodiment 1.
Table 3 embodiment 3: different sintering temperatures affect material property
Experiment sequence number sintering temperature (℃) specific surface area (m
2/ g) mean pore size (nm) pore volume (cm
3/ g) thing phase
Sample 13 500 349 4.88 048 γ-Al
2O
3
Sample 14 600 255 5.00 0.24 γ-Al
2O
3
Sample 15 700 236 5.38 0.32 γ-Al
2O
3
Sample 16 800 182 6.32 0.32 γ-Al
2O
3
Claims (3)
1. utilize waste aluminum sludge to prepare the method for activated alumina, it is characterized in that: production stage is:
(1) this mud is that the aluminium shape surface treating processes produces a large amount of waste liquids, and through the solid slag that sedimentation and filtration obtains, this mud main component is γ-AlOOH, Al (OH)
3With solid matter with amorphous body structure;
(2) adopt nitrate method: in through the dewatered sludge powder that grinds, adding dilute nitric acid solution and certain proportion dewatered sludge mixes and pugging, perhaps directly add water mixing pugging, form the plasticity walk, it is that 4-8mm is spherical that walk be may be formed into particle diameter, 100 ℃ of oven dry, after the drying, 400-900 ℃ of sintering, the sintered heat insulating time is 1-6 hour, obtains with γ-Al
2O
3Activated alumina for crystalline phase;
(3) Zhi Bei activated alumina outward appearance is that white and linen spherule, column or other are granular, and particle diameter is 3-7mm, its performance: specific surface area is 180-450m
2/ g, mean pore size is 3-7nm, pore volume is 0.15-0.8cm
3/ g, water-intake rate 〉=50%, folding strength 〉=70N/ ball.
2. the method for utilizing waste aluminum sludge to prepare activated alumina according to claim 1 is characterized in that: the dilute nitric acid solution of step (2) narration, the weight ratio of its concentrated nitric acid and water is 1: 1-1: 10.
3. the method for utilizing waste aluminum sludge to prepare activated alumina according to claim 1 is characterized in that: the dilute nitric acid solution of step (2) narration and the weight ratio of dewatered sludge are 1: 1-1: 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100140319A CN1305770C (en) | 2004-02-07 | 2004-02-07 | Method for preparing active aluminum oxide utilizing industrial sludge of aluminium section bar plant |
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|---|---|---|---|
| CNB2004100140319A CN1305770C (en) | 2004-02-07 | 2004-02-07 | Method for preparing active aluminum oxide utilizing industrial sludge of aluminium section bar plant |
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|---|---|
| CN1557714A true CN1557714A (en) | 2004-12-29 |
| CN1305770C CN1305770C (en) | 2007-03-21 |
Family
ID=34351248
Family Applications (1)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331805C (en) * | 2005-12-08 | 2007-08-15 | 福州大学 | Process for preparing aluminium oxide wear-resisting porcelain ball by industrial mud of aluminium section bar plant and preparation process thereof |
| CN100357181C (en) * | 2006-02-16 | 2007-12-26 | 福州大学 | Dilute nitric acid solution dipping and calcination process for regenerating waste active alumina |
| CN102319557A (en) * | 2011-09-01 | 2012-01-18 | 福州大学 | Active alumina/active carbon composite material and preparation method thereof |
| CN102351224A (en) * | 2011-07-01 | 2012-02-15 | 佛山科学技术学院 | Process for preparing active alumina from aluminum section industrial wastewater alkaline residues |
| CN102503208A (en) * | 2011-10-24 | 2012-06-20 | 广亚铝业有限公司 | Method for preparing fine powder additive for high-strength cement from waste water caustic sludge in aluminum profile industry |
| CN104512918A (en) * | 2013-09-27 | 2015-04-15 | 沈阳铝镁设计研究院有限公司 | Method for preparation of activated alumina from suspended solids in mother liquor |
| CN107971039A (en) * | 2017-11-30 | 2018-05-01 | 中海油天津化工研究设计院有限公司 | The method that alumina support or composite oxide carrier are prepared by organo-aluminium discarded object |
| US20220298068A1 (en) * | 2019-06-12 | 2022-09-22 | Ardex Group Gmbh | Process for Producing a Binder |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU615645A1 (en) * | 1976-11-09 | 1986-12-23 | Ордена Трудового Красного Знамени Институт Катализа Со Ан Ссср | Method of producing active granulated aluminium oxide |
| SU1658563A1 (en) * | 1989-08-28 | 1996-02-20 | Институт катализа СО АН СССР | Process for preparing aluminium oxide |
| RU2036146C1 (en) * | 1992-10-01 | 1995-05-27 | Анатолий Кузьмич Абрамов | Process for manufacture of active aluminum oxide granules |
| CN1043312C (en) * | 1993-06-24 | 1999-05-12 | 中国石油化工总公司 | Method for producing alumina carrier |
-
2004
- 2004-02-07 CN CNB2004100140319A patent/CN1305770C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331805C (en) * | 2005-12-08 | 2007-08-15 | 福州大学 | Process for preparing aluminium oxide wear-resisting porcelain ball by industrial mud of aluminium section bar plant and preparation process thereof |
| CN100357181C (en) * | 2006-02-16 | 2007-12-26 | 福州大学 | Dilute nitric acid solution dipping and calcination process for regenerating waste active alumina |
| CN102351224A (en) * | 2011-07-01 | 2012-02-15 | 佛山科学技术学院 | Process for preparing active alumina from aluminum section industrial wastewater alkaline residues |
| CN102319557A (en) * | 2011-09-01 | 2012-01-18 | 福州大学 | Active alumina/active carbon composite material and preparation method thereof |
| CN102503208A (en) * | 2011-10-24 | 2012-06-20 | 广亚铝业有限公司 | Method for preparing fine powder additive for high-strength cement from waste water caustic sludge in aluminum profile industry |
| CN104512918A (en) * | 2013-09-27 | 2015-04-15 | 沈阳铝镁设计研究院有限公司 | Method for preparation of activated alumina from suspended solids in mother liquor |
| CN104512918B (en) * | 2013-09-27 | 2016-12-07 | 沈阳铝镁设计研究院有限公司 | A kind of mother liquor floating material prepares the method for activated alumina |
| CN107971039A (en) * | 2017-11-30 | 2018-05-01 | 中海油天津化工研究设计院有限公司 | The method that alumina support or composite oxide carrier are prepared by organo-aluminium discarded object |
| CN107971039B (en) * | 2017-11-30 | 2020-10-30 | 中海油天津化工研究设计院有限公司 | Method for preparing alumina carrier or composite oxide carrier from organic aluminum waste |
| US20220298068A1 (en) * | 2019-06-12 | 2022-09-22 | Ardex Group Gmbh | Process for Producing a Binder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1305770C (en) | 2007-03-21 |
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Assignee: Fujian Minfa Aluminum Inc. Assignor: Fuzhou University Contract fulfillment period: 2009.5.11 to 2014.5.10 contract change Contract record no.: 2009350000086 Denomination of invention: Method for preparing active aluminum oxide utilizing industrial sludge of aluminium section bar plant Granted publication date: 20070321 License type: Exclusive license Record date: 2009.5.18 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.5.11 TO 2014.5.10; CHANGE OF CONTRACT Name of requester: MINFA ALUMINUM CO., LTD., FUJIAN PROVINCE Effective date: 20090518 |
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Granted publication date: 20070321 |