CN111732119A - Process for preparing aluminum ammonium sulfate by crystallization of two-stage leaching raffinate - Google Patents
Process for preparing aluminum ammonium sulfate by crystallization of two-stage leaching raffinate Download PDFInfo
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- CN111732119A CN111732119A CN202010654973.2A CN202010654973A CN111732119A CN 111732119 A CN111732119 A CN 111732119A CN 202010654973 A CN202010654973 A CN 202010654973A CN 111732119 A CN111732119 A CN 111732119A
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- aluminum
- ammonium sulfate
- ammonium
- sulfate
- crystallization
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- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000002425 crystallisation Methods 0.000 title claims abstract description 45
- 230000008025 crystallization Effects 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000002386 leaching Methods 0.000 title claims abstract description 16
- 239000012043 crude product Substances 0.000 claims abstract description 32
- 239000000047 product Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 230000008014 freezing Effects 0.000 claims abstract description 20
- 238000007710 freezing Methods 0.000 claims abstract description 20
- FOJJCOHOLNJIHE-UHFFFAOYSA-N aluminum;azane Chemical compound N.[Al+3] FOJJCOHOLNJIHE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 10
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 30
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical compound [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 239000011549 crystallization solution Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000001953 recrystallisation Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
- C01F7/765—Ammonium aluminium sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a process for preparing aluminum ammonium sulfate by crystallizing two-stage leaching raffinate, which comprises the following steps: (1) adding ammonium sulfate into the raffinate to perform ammonium-aluminum reaction, and crystallizing to obtain an aluminum-ammonium sulfate crude product; (2) adding a dissolving solution into the coarse product of the aluminum ammonium sulfate for dissolving and filtering, and performing vacuum crystallization to obtain a purer coarse product of the aluminum ammonium sulfate; (3) adding deionized water into the purer aluminum ammonium sulfate crude product for dissolving, and freezing and crystallizing to obtain a pure aluminum ammonium sulfate product. Firstly, obtaining an aluminum ammonium sulfate crude product through an ammonium-aluminum reaction; then, vacuum crystallization and filtration are carried out to obtain a crude product of aluminum ammonium sulfate with the purity of more than 80 percent; finally, the aluminum ammonium sulfate product with the concentration of about 99 percent is obtained by freezing, crystallizing and filtering. Therefore, the invention effectively recycles the aluminum in the second-stage leaching raffinate, and further purifies the recycled aluminum ammonium sulfate crude product so as to meet the requirements of industrial use.
Description
Technical Field
The invention belongs to the technical field of titanium ore recycling, and particularly relates to a process for preparing aluminum ammonium sulfate by crystallizing second-stage leaching raffinate.
Background
After the second-stage leaching solution is used for extracting titanium, the content of titanium and iron in the solution is low, and the preparation of aluminum ammonium sulfate with higher purity is facilitated. The prior art has added (NH) to the second leach raffinate4)2SO4The ammonium aluminum reaction is carried out, and after the reaction, the feed liquid is added into a crystallizer to carry out aluminum ammonium sulfate crystallization, however, the aluminum ammonium sulfate crystals prepared in the way are crude aluminum ammonium sulfate products containing many impurities, so that a crystallization and purification process of aluminum ammonium sulfate needs to be researched.
Disclosure of Invention
The invention provides a process for preparing aluminum ammonium sulfate by crystallizing two-stage leaching raffinate, which aims to overcome the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the process for preparing the ammonium aluminum sulfate by crystallizing the second-stage leaching raffinate comprises the following steps:
s1: adding ammonium sulfate into the raffinate to perform ammonium-aluminum reaction, and crystallizing to obtain an aluminum-ammonium sulfate crude product;
s2: adding a dissolving solution into the coarse product of the aluminum ammonium sulfate for dissolving and filtering, and performing vacuum crystallization to obtain a purer coarse product of the aluminum ammonium sulfate;
s3: adding deionized water into the purer aluminum ammonium sulfate crude product for dissolving, and freezing and crystallizing to obtain a pure aluminum ammonium sulfate product.
As a further description of the above technical solution: the step S1 includes the following sub-steps:
s11: heating raffinate, and adding ammonium sulfate according to a certain ammonium-aluminum molar ratio to react aluminum sulfate in the raffinate with the ammonium sulfate to generate aluminum ammonium sulfate;
s12: after the reaction, the feed liquid is added into a crystallizer to crystallize aluminum ammonium sulfate to obtain a crude product of the aluminum ammonium sulfate.
As a further description of the above technical solution: the heating temperature in the step S11 is 60-120 ℃; the reaction time in the step S11 is 10-60 min; the molar ratio of ammonium to aluminum in the step S11 is 1:1-1: 5.
As a further description of the above technical solution: the dissolving solution in step S2 is pure water.
As a further description of the above technical solution: the step S2 includes the following sub-steps:
s21: adding pure water into the crude product of the aluminum ammonium sulfate for dissolving;
s22: filtering the pure water solution to remove undissolved impurities;
s23: vacuum crystallizing the filtered solution to obtain a purer coarse product of the ammonium aluminum sulfate;
s24: the purer aluminum ammonium sulfate crude product is washed by washing water.
As a further description of the above technical solution: the step S2 further includes the following sub-steps:
s25: the washed filtrate is returned to step S21 for dissolution of the crude aluminum ammonium sulfate product.
As a further description of the above technical solution: the vacuum degree in the step S23 is 2000-2600 Pa.
As a further description of the above technical solution: the crystallization time in the step S23 is 30-90 min.
As a further description of the above technical solution: the step S3 includes the following sub-steps:
s31: adding deionized water into the purer coarse product of the aluminum ammonium sulfate for dissolving;
s32: freezing and crystallizing the deionized water solution to obtain a crystallization solution;
s33: filtering the crystallization solution to obtain a pure aluminum ammonium sulfate product and a filtrate;
s34: the filtrate is returned to step S24 and used as washing water.
As a further description of the above technical solution: the freezing and crystallizing temperature in the step S32 is-30-15 ℃; the freezing and crystallizing time in the step S32 is 30-90 min.
The invention has the following beneficial effects:
firstly, obtaining an aluminum ammonium sulfate crude product through an ammonium-aluminum reaction; then, vacuum crystallization and filtration are carried out to obtain a crude product of aluminum ammonium sulfate with the purity of more than 80 percent; finally, the aluminum ammonium sulfate product with the concentration of about 99 percent is obtained by freezing, crystallizing and filtering. Therefore, the invention effectively recycles the aluminum in the second-stage leaching raffinate, and further purifies the recycled aluminum ammonium sulfate crude product so as to meet the requirements of industrial use.
Drawings
FIG. 1 is a flow chart of a process for preparing ammonium aluminum sulfate by two-stage leaching raffinate crystallization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in figure 1, the process for preparing the ammonium aluminum sulfate by the crystallization of the two-stage leaching raffinate comprises the following steps:
(1) adding ammonium sulfate into the raffinate to perform ammonium-aluminum reaction, and crystallizing to obtain an aluminum-ammonium sulfate crude product;
(2) adding a dissolving solution into the coarse product of the aluminum ammonium sulfate for dissolving and filtering, and performing vacuum crystallization to obtain a purer coarse product of the aluminum ammonium sulfate;
(3) adding deionized water into the purer aluminum ammonium sulfate crude product for dissolving, and freezing and crystallizing to obtain a pure aluminum ammonium sulfate product.
Firstly, obtaining an aluminum ammonium sulfate crude product through an ammonium-aluminum reaction; then, vacuum crystallization and filtration are carried out to obtain a crude product of aluminum ammonium sulfate with the purity of more than 80 percent; finally, the aluminum ammonium sulfate product with the concentration of about 99 percent is obtained by freezing, crystallizing and filtering. Therefore, the invention effectively recycles the aluminum in the second-stage leaching raffinate, and further purifies the recycled aluminum ammonium sulfate crude product so as to meet the requirements of industrial use.
In this embodiment, the step (1) includes the following sub-steps:
(11) heating raffinate, and adding ammonium sulfate according to a certain ammonium-aluminum molar ratio to react aluminum sulfate in the raffinate with the ammonium sulfate to generate aluminum ammonium sulfate;
(12) after the reaction, the feed liquid is added into a crystallizer for aluminum ammonium sulfate crystallization, and then the crude product of the aluminum ammonium sulfate and the crystallization tail liquid are obtained by filtration.
In the present embodiment, the heating temperature in step (11) is 60-120 ℃, preferably, the heating temperature in step (11) is 80 ℃; the reaction time in the step (11) is 10-60min, and preferably, the reaction time in the step (11) is 30 min; the molar ratio of ammonium to aluminum in the step (11) is 1:1-1:5, and preferably, the molar ratio of ammonium to aluminum in the step (11) is 1: 3.
In this embodiment, the dissolving solution in the step (2) is pure water.
In this embodiment, the step (2) includes the following sub-steps:
(21) adding pure water into the crude product of the aluminum ammonium sulfate for dissolving;
(22) filtering the pure water solution to remove undissolved impurities;
(23) carrying out vacuum crystallization and filtration on the filtered solution to obtain a purer coarse product of the ammonium aluminum sulfate;
(24) the purer aluminum ammonium sulfate crude product is washed by washing water.
(25) And (5) returning the washed filtrate to the step (21) for dissolving the crude product of the aluminum ammonium sulfate.
In the present embodiment, the vacuum degree in the step (23) is 2000-2600Pa, preferably, the vacuum degree in the step (23) is 2400 Pa; the crystallization time in the step (23) is 30-90min, and preferably, the crystallization time in the step (23) is 60 min.
In this embodiment, the step (3) includes the following sub-steps:
(31) adding deionized water into the purer coarse product of the aluminum ammonium sulfate for dissolving;
(32) freezing and crystallizing the deionized water solution to obtain a crystallization solution;
(33) filtering the crystallization solution to obtain a pure aluminum ammonium sulfate product and a filtrate;
(34) the filtrate is returned to step (24) for use as wash water.
In this embodiment, the freezing crystallization temperature in the step (32) is-30-15 ℃; the freezing and crystallizing time in the step (32) is 30-90min, and preferably, the freezing and crystallizing time in the step (32) is 60 min.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
As shown in figure 1, after the titanium is extracted from the second-stage leaching solution, the content of titanium and iron in the solution is low, and the preparation of aluminum ammonium sulfate with higher purity is facilitated. Heating the leaching solution to 80 ℃, and adding (NH) according to the molar ratio of ammonium to aluminum of 1:34)2SO4And (3) carrying out an ammonium-aluminum reaction, maintaining the reaction temperature at 80 ℃, reacting for 30min, adding the feed liquid into a crystallizer after the reaction for carrying out aluminum ammonium sulfate crystallization, and then filtering to obtain an aluminum ammonium sulfate crystallization crude product. The purification of the crude product of the ammonium aluminum sulfate crystallization is carried out by two times, wherein the first time adopts vacuum crystallization (namely primary recrystallization), the vacuum degree of a system is controlled to be 2400Pa, the crystallization time is 60min, more than 80 percent of the crude product of the ammonium aluminum sulfate is obtained by filtering, the second time adopts freezing crystallization (namely secondary recrystallization), the crystallization temperature is controlled to be less than or equal to 15 ℃, the crystallization time is 60min, and about 99 percent of the ammonium aluminum sulfate product is obtained by filtering.
Dissolving the first vacuum crystallization product by using deionized water, performing second freezing crystallization (namely, secondary recrystallization), and performing crystallization and purification twice to obtain the final aluminum ammonium sulfate product. The second freezing crystallization filtrate is returned as the washing water of the first vacuum crystallization product, the washed liquid is used for dissolving the aluminum ammonium sulfate crude product, insoluble impurities are filtered after the aluminum ammonium sulfate crude product is dissolved to carry out first vacuum crystallization (namely, primary recrystallization), and the first vacuum crystallization filtrate is returned as dilution filtration make-up water of leached ore pulp to form a closed circuit.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. The process for preparing the ammonium aluminum sulfate by crystallizing the second-stage leaching raffinate is characterized by comprising the following steps of:
s1: adding ammonium sulfate into the raffinate to perform ammonium-aluminum reaction, and crystallizing to obtain an aluminum-ammonium sulfate crude product;
s2: adding a dissolving solution into the coarse product of the aluminum ammonium sulfate for dissolving and filtering, and performing vacuum crystallization to obtain a purer coarse product of the aluminum ammonium sulfate;
s3: adding deionized water into the purer aluminum ammonium sulfate crude product for dissolving, and freezing and crystallizing to obtain a pure aluminum ammonium sulfate product.
2. The process for preparing ammonium aluminum sulfate by crystallization of two-stage leach raffinate according to claim 1, wherein the step S1 comprises the following sub-steps:
s11: heating raffinate, and adding ammonium sulfate according to a certain ammonium-aluminum molar ratio to react aluminum sulfate in the raffinate with the ammonium sulfate to generate aluminum ammonium sulfate;
s12: after the reaction, the feed liquid is added into a crystallizer to crystallize aluminum ammonium sulfate to obtain a crude product of the aluminum ammonium sulfate.
3. The process for preparing ammonium aluminum sulfate by crystallization of two-stage leach raffinate according to claim 2, wherein the heating temperature in the step S11 is 60-120 ℃; the reaction time in the step S11 is 10-60 min; the molar ratio of ammonium to aluminum in the step S11 is 1:1-1: 5.
4. The process for preparing ammonium aluminum sulfate by crystallization of two-stage leach raffinate according to claim 1, wherein the dissolving solution in the step S2 is pure water.
5. The process for preparing ammonium aluminum sulfate by crystallization of two-stage leach raffinate according to claim 4, wherein the step S2 comprises the following sub-steps:
s21: adding pure water into the crude product of the aluminum ammonium sulfate for dissolving;
s22: filtering the pure water solution to remove undissolved impurities;
s23: vacuum crystallizing the filtered solution to obtain a purer coarse product of the ammonium aluminum sulfate;
s24: the purer aluminum ammonium sulfate crude product is washed by washing water.
6. The process for preparing aluminum ammonium sulfate by crystallization of two-stage leach raffinate according to claim 5, wherein the step S2 further comprises the following sub-steps:
s25: the washed filtrate is returned to step S21 for dissolution of the crude aluminum ammonium sulfate product.
7. The process for preparing ammonium aluminum sulfate by crystallization of two-stage leach raffinate as claimed in claim 5, wherein the vacuum degree in the step S23 is 2000-2600 Pa.
8. The process for preparing ammonium aluminum sulfate by two-stage leaching raffinate crystallization in claim 5, wherein the crystallization time in the step S23 is 30-90 min.
9. The process for preparing ammonium aluminum sulfate by crystallization of two-stage leach raffinate according to claim 1, wherein the step S3 comprises the following sub-steps:
s31: adding deionized water into the purer coarse product of the aluminum ammonium sulfate for dissolving;
s32: freezing and crystallizing the deionized water solution to obtain a crystallization solution;
s33: filtering the crystallization solution to obtain a pure aluminum ammonium sulfate product and a filtrate;
s34: the filtrate is returned to step S24 and used as washing water.
10. The process for preparing ammonium aluminum sulfate by crystallization of two-stage leach raffinate according to claim 9, wherein the freezing and crystallizing temperature in the step S32 is-30-15 ℃; the freezing and crystallizing time in the step S32 is 30-90 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114250367A (en) * | 2021-12-29 | 2022-03-29 | 五矿稀土江华有限公司 | Method for comprehensively recovering valuable elements in ionic rare earth impurity removal slag |
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