CN108217688B - Deep hydrolysis method for aluminum nitride in aluminum ash - Google Patents
Deep hydrolysis method for aluminum nitride in aluminum ash Download PDFInfo
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- CN108217688B CN108217688B CN201810074432.5A CN201810074432A CN108217688B CN 108217688 B CN108217688 B CN 108217688B CN 201810074432 A CN201810074432 A CN 201810074432A CN 108217688 B CN108217688 B CN 108217688B
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- aluminum
- aluminum ash
- aluminum nitride
- ash
- hydrolysis
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 51
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 39
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 28
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 239000012065 filter cake Substances 0.000 claims abstract description 9
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 5
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract 1
- 238000002386 leaching Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/026—Preparation of ammonia from inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/242—Preparation from ammonia and sulfuric acid or sulfur trioxide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a deep hydrolysis method of aluminum nitride in aluminum ash, which comprises the following steps: 1) crushing the aluminum ash to be less than 10mm, heating the aluminum ash to a certain temperature, and uniformly mixing the aluminum ash and water according to a certain proportion; 2) grinding and hydrolyzing the obtained high-temperature slurry, and collecting ammonia gas generated by hydrolysis to obtain corresponding ammonia water or ammonium salt; 3) dehydrating and filtering the hydrolyzed slurry to obtain a filter cake and a filtrate; and circularly enriching the filtrate and evaporating to recover the industrial salt. The method strengthens the hydrolysis process of the aluminum nitride through high-temperature grinding, realizes the deep hydrolysis of the aluminum nitride, simultaneously realizes the recovery of ammonia, and opens up a new way for the harmless and resource utilization of the aluminum nitride in the aluminum ash.
Description
Technical Field
The invention belongs to the technical field of electrolytic aluminum solid waste treatment, and particularly relates to a deep hydrolysis method of aluminum nitride in aluminum ash.
Background
The aluminum ash is floating slag on the surface of an aluminum melt in the electrolytic aluminum and aluminum smelting process, is in a loose ash shape, has great threat to the surrounding environment due to containing a large amount of aluminum nitride and fluoride, and is listed as dangerous waste by the state. China is a big country for producing electrolytic aluminum, accounts for more than half of the world electrolytic aluminum output, and produces more than 150 million tons of waste aluminum ash every year. Therefore, the harmless disposal method of the waste aluminum ash becomes one of the problems to be solved urgently in the environmental protection work of China.
At present, the content of aluminum nitride is generally 1-30% according to different processes of aluminum ash production, and because the aluminum nitride is unstable, hydrolysis reaction can occur when the aluminum nitride meets water to release ammonia gas, so that serious environmental pollution is caused to the surrounding environment, and the reaction is used for producing ammonia in the past.
AlN+3H2O=Al(OH)3+NH3
At present, the domestic aluminum ash is mainly stockpiled, and aluminum nitride in the aluminum ash is easy to absorb water to generate hydrolysis reaction and release a large amount of ammonia gas. The hydrolysis speed of the aluminum nitride is relatively slow at normal temperature, the hydrolysis period is long, and the continuous harm to the environment is large, so that the development of the rapid deep hydrolysis method of the aluminum nitride has important significance for harmless treatment of the aluminum nitride in the aluminum ash.
Disclosure of Invention
Aiming at the defects in the prior art, the invention mainly aims to solve the problems of low hydrolysis speed, long period, incomplete hydrolysis and the like of aluminum nitride in aluminum ash in a natural state, provides a deep hydrolysis method of aluminum nitride in aluminum ash, and provides an effective way for harmless treatment of aluminum nitride in aluminum ash.
The method for deeply hydrolyzing the aluminum nitride in the aluminum ash provided by the invention is characterized in that the hydrolysis speed of the aluminum nitride is increased by increasing the hydrolysis temperature of the aluminum ash raw material; continuously stripping aluminum hydroxide generated by the hydrolysis of the surface of the aluminum nitride through continuously wetting powder, and maintaining the high-speed hydrolysis of the aluminum nitride; the ammonia generated by the hydrolysis of the aluminum nitride is recovered, so that the harmless treatment and resource utilization of the aluminum nitride in the aluminum ash are realized.
The method for deeply hydrolyzing the aluminum nitride in the aluminum ash comprises the following steps of:
1) crushing the aluminum ash to be less than 10 mm;
2) heating the aluminum ash obtained in the step 1) to more than 100 ℃, and then uniformly mixing the aluminum ash with water according to a certain proportion to obtain high-temperature slurry; 3) grinding and hydrolyzing the high-temperature slurry obtained in the step 2), and collecting ammonia gas generated by hydrolysis;
4) absorbing the ammonia gas obtained in the step 3) to obtain corresponding ammonia water or ammonium salt;
5) dehydrating and filtering the slurry hydrolyzed in the step 4) to obtain a filter cake and a filtrate;
6) circularly enriching the filtrate obtained in the step 5), and evaporating to recover the industrial salt.
Preferably, in the step 2), the aluminum ash is heated to 100-300 DEG C
Preferably, in the step 2), the mass ratio of the aluminum ash to the water is 3: 1-1: 3.
Preferably, in the step 4), the grinding is wet sealing grinding, and the grinding time is 30-90 min.
Preferably, in step 4), the medium used for ammonia absorption is water, hydrochloric acid or sulfuric acid.
Compared with the hydrolysis in a normal-temperature stirring tank, the method for deeply hydrolyzing the aluminum nitride in the aluminum ash has the following obvious advantages:
1) according to the invention, through the hydrolysis process of the high-temperature powder reinforced aluminum nitride, more than 98% of aluminum nitride can be hydrolyzed within 60min, and the hydrolysis efficiency of the aluminum nitride is greatly improved.
2) The ammonia water and ammonium salt are produced by absorbing the hydrolyzed ammonia gas, so that the resource utilization of the aluminum nitride can be realized.
Detailed Description
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. Unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features. The description is only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
A typical aluminum ash composition is as follows
Composition (I) | Al2O3 | SiO2 | Fe | AlN | Na |
Content/% | 73.65 | 6.22 | 5.16 | 11.41 | 3.12 |
Example 1
Crushing 1kg of aluminum ash to below 10mm by using a back-impact crusher, heating the aluminum ash to 200 ℃, carrying out wet sealing grinding leaching on the aluminum ash and water according to the proportion of 3:1, absorbing ammonia gas generated in the grinding process by using water to obtain ammonia water, grinding ores for 30min, carrying out plate-and-frame filter pressing to obtain a filter cake and a filtrate, analyzing the content of aluminum nitride in the filter cake, and finding that the content of aluminum nitride hydrolysis is 99.21%, and evaporating the filtrate to obtain industrial salt.
Example 2
Crushing 1kg of aluminum ash to below 10mm by using a back-impact crusher, heating the aluminum ash to 300 ℃, carrying out wet sealing grinding leaching on the aluminum ash and water according to the proportion of 1:3, absorbing ammonia gas generated in the grinding process by using hydrochloric acid to obtain ammonium chloride, grinding ores for 90min, carrying out plate-and-frame filter pressing to obtain a filter cake and a filtrate, analyzing the content of aluminum nitride in the filter cake, and finding out that the content of aluminum nitride is 99.31%, and evaporating the filtrate to obtain industrial salt.
Example 3
Crushing 1kg of aluminum ash to below 10mm by using a back-impact crusher, heating the aluminum ash to 100 ℃, carrying out wet sealing grinding and leaching on the aluminum ash and hot water according to the proportion of 2:1, absorbing ammonia gas generated in the grinding process by using sulfuric acid to obtain ammonium sulfate, grinding ores for 60min, carrying out plate-and-frame filter pressing to obtain a filter cake and a filtrate, analyzing the content of aluminum nitride in the filter cake, and finding that the content of aluminum nitride hydrolysis is 99.51%, and evaporating the filtrate to obtain industrial salt.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (3)
1. A method for deep hydrolysis of aluminum nitride in aluminum ash, the method comprising the steps of:
1) crushing the aluminum ash to be less than 10 mm;
2) heating the aluminum ash obtained in the step 1) to 200-300 ℃, and then uniformly mixing the aluminum ash with water according to a certain proportion to obtain high-temperature slurry;
3) grinding and hydrolyzing the high-temperature slurry obtained in the step 2), and collecting ammonia gas generated by hydrolysis;
4) absorbing the ammonia gas obtained in the step 3) to obtain corresponding ammonia water or ammonium salt;
5) dehydrating and filtering the slurry hydrolyzed in the step 3) to obtain a filter cake and a filtrate;
6) circularly enriching the filtrate obtained in the step 5), and evaporating to recover industrial salt;
in the step 4), the grinding is wet sealing grinding, and the grinding time is 30 min.
2. The method for deeply hydrolyzing the aluminum nitride in the aluminum ash according to claim 1, wherein in the step 2), the mass ratio of the aluminum ash to the water is 3:1 to 1: 3.
3. The method for deeply hydrolyzing aluminum nitride in aluminum ash as claimed in claim 1, wherein the medium used for ammonia absorption in step 4) is water, hydrochloric acid or sulfuric acid.
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CN201810074432.5A CN108217688B (en) | 2018-01-25 | 2018-01-25 | Deep hydrolysis method for aluminum nitride in aluminum ash |
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CN110314923B (en) * | 2019-07-12 | 2021-01-22 | 郑州中科新兴产业技术研究院 | Method for strengthening desalination and denitrification of aluminum ash |
CN110723746A (en) * | 2019-11-04 | 2020-01-24 | 湖南绿脉环保科技有限公司 | Harmless treatment method for aluminum ash |
CN112978778A (en) * | 2019-12-13 | 2021-06-18 | 南京理工大学 | Method for preparing polyaluminum chloride by aluminum mortar method |
CN113716591A (en) * | 2021-08-30 | 2021-11-30 | 河南同本科技有限公司 | Aluminum ash recycling method |
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SI9700229A (en) * | 1997-09-05 | 1999-04-30 | Inštitut "Jožef Stefan" | Process for protection of aluminium nitride powder against hydrolysis |
CN107555447A (en) * | 2017-08-10 | 2018-01-09 | 中国铝业股份有限公司 | A kind of method of the innoxious comprehensive utilization of Quadratic aluminum dust |
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