CN100540474C - From sodium aluminate solution, extract the method for molybdenum - Google Patents
From sodium aluminate solution, extract the method for molybdenum Download PDFInfo
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- CN100540474C CN100540474C CNB2007100155426A CN200710015542A CN100540474C CN 100540474 C CN100540474 C CN 100540474C CN B2007100155426 A CNB2007100155426 A CN B2007100155426A CN 200710015542 A CN200710015542 A CN 200710015542A CN 100540474 C CN100540474 C CN 100540474C
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- molybdenum
- sodium aluminate
- aluminate solution
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- crystallisation
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 62
- 239000011733 molybdenum Substances 0.000 title claims abstract description 62
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910001388 sodium aluminate Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000284 extract Substances 0.000 title description 5
- 239000000243 solution Substances 0.000 claims abstract description 47
- 238000002425 crystallisation Methods 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000010413 mother solution Substances 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 18
- 230000008020 evaporation Effects 0.000 claims abstract description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 10
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 9
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 9
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 9
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 4
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract 2
- 239000003513 alkali Substances 0.000 claims description 26
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052799 carbon Inorganic materials 0.000 abstract description 13
- 239000002699 waste material Substances 0.000 abstract description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 235000011089 carbon dioxide Nutrition 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229940001593 sodium carbonate Drugs 0.000 description 2
- XYQRXRFVKUPBQN-UHFFFAOYSA-L Sodium carbonate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]C([O-])=O XYQRXRFVKUPBQN-UHFFFAOYSA-L 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229940018038 sodium carbonate decahydrate Drugs 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to a kind of method of from sodium aluminate solution, extracting molybdenum, in sodium aluminate solution, feed carbon dioxide gas, sodium aluminate solution is carried out thorough carbonating to be decomposed, filter and remove aluminium hydroxide, yellow soda ash is removed in carbon mother liquid evaporation and crystallisation by cooling, make the molybdenum in the crystalline mother solution obtain enrichment, to enrichment add acid in the crystalline mother solution of molybdenum, adding ammonium, to carry out acid heavy, can be settled out thick ammonium molybdate.Advantages of simple, simple and easy to do, utilize the inventive method that the molybdenum in the sodium aluminate solution is reclaimed well, turn waste into wealth, realized the comprehensive utilization of resource, remarkable in economical benefits.
Description
Technical field
The present invention relates to a kind of method of from sodium aluminate solution, extracting molybdenum, make the molybdenum in the alumina base spent catalyst obtain reclaiming.
Background technology
When containing the alumina base spent catalyst of molybdenum with the method processing of joining alkaline sintering, the molybdenum that can contain 0.5-4g/l in the sodium aluminate solution that the grog stripping obtains, molybdenum is the higher rare metal of a kind of value ratio, will not wasted if do not extract, and is very unfortunate.
Usually, aluminium mainly is to extract from the ore that contains molybdenum, also have from the spent catalyst that contains molybdenum and to extract molybdenum, but the solution that contains molybdenum that these methods obtain all is tart, neutral or weakly alkaline, does not also see the report that extracts molybdenum from the strong alkali solution (being sodium aluminate solution) that contains a large amount of aluminum oxide at present.
Summary of the invention
The object of the present invention is to provide a kind of method of from sodium aluminate solution, extracting molybdenum, make the molybdenum in the sodium aluminate solution obtain reclaiming, turn waste into wealth, realize the comprehensive utilization of resource.
The method of from sodium aluminate solution, extracting molybdenum of the present invention, at first in sodium aluminate solution, feed carbon dioxide gas, sodium aluminate solution is carried out carbonating to be decomposed, filter and remove aluminium hydroxide, again yellow soda ash is removed in carbon mother liquid evaporation and crystallisation by cooling, is made the molybdenum in the crystalline mother solution obtain enrichment, then to enrichment add acid in the crystalline mother solution of molybdenum, add ammonium salt or ammoniacal liquor and carry out acid and sink, can be settled out thick ammonium molybdate, thereby make molybdenum wherein obtain recovery.
The aluminum oxide residual quantity preferably is less than or equal to 1g/l in the decomposition nut liquid after carbonating is decomposed.
If the molybdenum content of initial aluminum acid sodium solution is lower, the molybdenum content that perhaps requires final solution is than higher, and the step that the evaporation of carbonating decomposition nut liquid, crystallisation by cooling are handled can repeatedly be carried out several times more.
Acid is sunk when handling, and control PH scope is that 0.8-2.5 is suitable.
Suitable requirement, preferably full alkali reaches 150-300g/l in the sodium aluminate solution, contains the molybdenum amount and reaches 0.5-4g/l.
Suitable control, molybdenum content reaches 30-200g/l in the crystalline mother solution before acid is heavy, and full alkali reaches 50-100g/l.
The inventive method is applicable to from alkaline sodium aluminate solution extracts molybdenum.At first feed carbon dioxide gas in sodium aluminate solution, sodium aluminate solution is carried out thorough carbonating decompose, obtain aluminium hydroxide, thoroughly remove the aluminum oxide in the solution, the caustic alkali in the solution also all changes carbonic acid alkali into simultaneously, and molybdenum has then been stayed in the solution.Then sodium carbonate solution being carried out crystallisation by cooling, separate out a part of yellow soda ash, is the yellow soda ash that contains ten crystal water owing to what separate out, can take away the large quantity of moisture in the solution, so the content of molybdenum is also concentrated simultaneously, improves in the solution.Mother liquor after the crystallization continues evaporation, crystallisation by cooling, further separates out yellow soda ash, further improves the content of molybdenum simultaneously.If the molybdenum content of initial aluminum acid sodium solution is lower, the molybdenum content that perhaps requires final solution is than higher, and the step of evaporation and crystallisation by cooling can be carried out several times more.Through pervaporation and crystallisation by cooling, can obtain containing molybdenum 30-200g/l, the sodium carbonate solution of full alkali 50-100g/l, this solution adds acid solution, and then adds ammonium salt or ammoniacal liquor, and acid is sunk and is obtained thick ammonium molybdate, and thick ammonium molybdate can further be purified and be obtained pure ammonium molybdate.
The inventive method advantages of simple, simple and easy to do, utilize the inventive method that the molybdenum in the sodium aluminate solution is reclaimed well, turn waste into wealth, realized the comprehensive utilization of resource, remarkable in economical benefits.
Description of drawings
Fig. 1 is the process flow diagram of the inventive method.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Contain full alkali 150g/l, aluminum oxide 140g/l, the sodium aluminate solution of molybdenum 0.5g/l feeds the thorough carbon branch of carbonic acid gas, and obtaining composition is full alkali 160g/l, aluminum oxide 0.2g/l, the carbon mother liquid of molybdenum 0.6g/l; The carbon mother liquid crystallization and evaporation filters, and obtains full alkali 240g/l, the mother liquid evaporation of molybdenum 1.5g/l; Mother liquid evaporation is cooled to 10 ℃, and crystallisation by cooling filters, and obtains full alkali 80g/l, the crystalline mother solution of molybdenum 3.75g/l; The crystallisation by cooling mother liquor evaporates once more, obtains full alkali 240g/l, the mother liquid evaporation of molybdenum 11.25g/l; Mother liquid evaporation is cooled to 5 ℃, and crystallisation by cooling filters, and obtains full alkali 50g/l, the crystalline mother solution of molybdenum 33.75g/l.It is acid that crystalline mother solution adds hydrochloric acid accent pH value, and transferring pH value is 0.8, adds ammonium chloride and obtains thick ammonium molybdate.
Embodiment 2
Contain full alkali 220g/l, aluminum oxide 200g/l, the sodium aluminate solution of molybdenum 2g/l feeds the thorough carbon branch of carbonic acid gas, and obtaining composition is full alkali 230g/l, aluminum oxide 1g/l, the carbon mother liquid of molybdenum 2.4g/l; Carbon mother liquid is cooled to 10 ℃, and crystallisation by cooling filters, and obtains full alkali 80g/l, the crystalline mother solution of molybdenum 6g/l; The crystallisation by cooling mother liquor evaporates once more, obtains full alkali 240g/l, the mother liquid evaporation of molybdenum 18g/l; Mother liquid evaporation is cooled to 5 ℃, and crystallisation by cooling filters, and obtains full alkali 50g/l, the crystalline mother solution of molybdenum 54g/l.It is acid that crystalline mother solution adds hydrochloric acid accent pH value, and transferring pH value is 2, adds ammonium chloride and obtains thick ammonium molybdate.
Embodiment 3
Contain full alkali 240g/l, aluminum oxide 220g/l, the sodium aluminate solution of molybdenum 4g/l feeds the thorough carbon branch of carbonic acid gas, and obtaining composition is full alkali 240g/l, aluminum oxide 1g/l, the carbon mother liquid of molybdenum 4.6g/l; Carbon mother liquid is cooled to 10 ℃, and crystallisation by cooling filters, and obtains full alkali 80g/l, the crystalline mother solution of aluminium 11.5g/l; The crystallisation by cooling mother liquor is crystallization and evaporation once more, filters, and obtains full alkali 240g/l, the mother liquid evaporation of molybdenum 57.5g/l; Mother liquid evaporation is cooled to 5 ℃, and crystallisation by cooling filters, and obtains full alkali 50g/l, the crystalline mother solution of molybdenum 172.5g/l.It is acid that crystalline mother solution adds hydrochloric acid accent pH value, and transferring pH value is 2.5, adds ammonium chloride and obtains thick ammonium molybdate.
Embodiment 4
Contain molybdenum 2.8g/l, the sodium aluminate solution of full alkali 230g/l carries out thorough carbonating and decomposes, the residual aluminum oxide 1g/l of carbon mother liquid, and contain molybdenum 3.6g/l.Carbon mother liquid is separated out the part Sodium carbonate decahydrate at 15 ℃ of following crystallisation by cooling, obtains full alkali 85g/l, contains the crystalline mother solution of molybdenum 10g/l.One times of crystalline mother solution evaporation concentration, molybdenum content reaches 20g/l, and the solution after the evaporation is crystallisation by cooling once more, obtains containing the crystalline mother solution of molybdenum 53g/l.This solution adds hydrochloric acid, and transferring pH value is 1.2, adds ammonium chloride again and obtains thick many ammonium molybdates.
Claims (5)
1, a kind of method of from sodium aluminate solution, extracting molybdenum, it is characterized in that in sodium aluminate solution, feeding carbon dioxide gas, sodium aluminate solution is carried out thorough carbonating to be decomposed, filter and remove aluminium hydroxide, yellow soda ash is removed in carbonating decomposition nut liquid evaporation and crystallisation by cooling, is made the aluminium in the crystalline mother solution obtain enrichment, to enrichment add acid in the crystalline mother solution of molybdenum, add ammonium and carry out the heavy processing of acid, control pH scope 0.8-2.5 can be settled out thick ammonium molybdate.
2, the method for extracting molybdenum from sodium aluminate solution according to claim 1 is characterized in that the aluminum oxide residual quantity is less than or equal to 1g/l in the decomposition nut liquid after carbonating is decomposed.
3, the method for extracting molybdenum from sodium aluminate solution according to claim 2 is characterized in that the carbonating decomposition nut liquid evaporates repeatedly, crystallisation by cooling is handled.
4, according to claim 1, the 2 or 3 described methods of extracting molybdenum from sodium aluminate solution, it is characterized in that full alkali is 150-300g/l in the sodium aluminate solution, containing the molybdenum amount is 0.5-4g/l.
5, the method for extracting molybdenum from sodium aluminate solution according to claim 4 is characterized in that molybdenum content 30-200g/l in the heavy preceding crystalline mother solution of acid, and full alkali is 50-100g/l.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100155426A CN100540474C (en) | 2007-05-15 | 2007-05-15 | From sodium aluminate solution, extract the method for molybdenum |
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| CNB2007100155426A CN100540474C (en) | 2007-05-15 | 2007-05-15 | From sodium aluminate solution, extract the method for molybdenum |
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| CN101049967A CN101049967A (en) | 2007-10-10 |
| CN100540474C true CN100540474C (en) | 2009-09-16 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4657745A (en) * | 1986-03-31 | 1987-04-14 | Chemical & Metal Industries, Inc. | Value recovery from spent alumina-base catalyst |
| US4666685A (en) * | 1986-05-09 | 1987-05-19 | Amax Inc. | Selective extraction of molybdenum and vanadium from spent catalysts by oxidative leaching with sodium aluminate and caustic |
| CN1258754A (en) * | 1998-12-30 | 2000-07-05 | 王犇 | Recovery process of waste cobalt-molybdenum catalyst |
| CN1544666A (en) * | 2003-11-14 | 2004-11-10 | 沈阳嘉禾冶金炉料有限公司 | Method for recovering nickel and aluminum from waste aluminum based nickel-containing catalyst |
| CN1865460A (en) * | 2005-05-20 | 2006-11-22 | 中南大学 | Method for extracting vanadium,molybdenum,nickel,cobalt,aluminium from waste aluminium base catalyst |
-
2007
- 2007-05-15 CN CNB2007100155426A patent/CN100540474C/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4657745A (en) * | 1986-03-31 | 1987-04-14 | Chemical & Metal Industries, Inc. | Value recovery from spent alumina-base catalyst |
| US4666685A (en) * | 1986-05-09 | 1987-05-19 | Amax Inc. | Selective extraction of molybdenum and vanadium from spent catalysts by oxidative leaching with sodium aluminate and caustic |
| CN1258754A (en) * | 1998-12-30 | 2000-07-05 | 王犇 | Recovery process of waste cobalt-molybdenum catalyst |
| CN1544666A (en) * | 2003-11-14 | 2004-11-10 | 沈阳嘉禾冶金炉料有限公司 | Method for recovering nickel and aluminum from waste aluminum based nickel-containing catalyst |
| CN1865460A (en) * | 2005-05-20 | 2006-11-22 | 中南大学 | Method for extracting vanadium,molybdenum,nickel,cobalt,aluminium from waste aluminium base catalyst |
Non-Patent Citations (2)
| Title |
|---|
| 废铝基催化剂综合利用新工艺研究. 冯其明等.金属矿山，第12期. 2005 |
| 废铝基催化剂综合利用新工艺研究. 冯其明等.金属矿山，第12期. 2005 * |
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Effective date of registration: 20071026 Address after: No. 62 North Main Street, Beijing, Xizhimen Applicant after: Aluminum Corporation of China Limited Address before: No. five, 1 km road, Zhangdian District, Shandong, Zibo Applicant before: Shandong Aluminium Industry Co., Ltd. |
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