CN105803207B - A kind of recycling reuse method of Bayer process red mud - Google Patents
A kind of recycling reuse method of Bayer process red mud Download PDFInfo
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- CN105803207B CN105803207B CN201610219802.0A CN201610219802A CN105803207B CN 105803207 B CN105803207 B CN 105803207B CN 201610219802 A CN201610219802 A CN 201610219802A CN 105803207 B CN105803207 B CN 105803207B
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- acid
- red mud
- bayer process
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- 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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- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of recycling reuse method of Bayer process red mud, the specific steps are：It is sieved after Bayer process red mud is dried, it is 1 in mass ratio to screen out 400 800 hot eyes mud sample product with sodium hydroxide:0.5 1 are uniformly mixed after 800 DEG C of constant temperature calcining 4h, it takes out sample comminution and is uniformly mixed with water, 1 2h of heating stirring in 100 DEG C of water-bath, filtering, it is 10.5 that filtrate, which adds in hydrofluoric acid and adjusts pH, it is uniformly mixed to be placed in kettle of refining and 6 48h are baked in 100 DEG C obtains zeolite, filter cake is dried after repeatedly washing, and the mixed acid of the sample after drying and citric acid and acetic acid is added to the extraction and separation that 20 40min are extracted in micro-wave digestion abstraction instrument and complete rare earth element.The content of rare earth that the present invention is extracted through extraction processing from Bayer process red mud sample significantly increases, and improves the utilization rate of mineral resources, and environmental protection while is also beneficial to the recycling of Bayer process red mud.
Description
Technical field
The invention belongs to the recycling reutilization technology fields of solid waste dangerous in environmental protection, and in particular to a kind of
The recycling reuse method of Bayer process red mud.
Background technology
It is well known that rare-earth like mine and other common metal mineral facies ratios, not only its reserve is considerably less, but also very
Difficulty is detached from raw ore, therefore above-mentioned rare earth metal is rare mineral, and price is largely very high.Conversely, because
Various electronic equipments etc. are highly desirable to rare earth metal, therefore growing day by day for the needs of rare earth metal.Bayer process red mud
The content of middle rare earth metal is relatively high, and red mud largely stores up not only land occupation, waste of resource, but also brings environment dirty
Dye and the hidden loyalty of safety.The comprehensive utilization of Bayer process red mud is to solve the basic plan of its environmental pollution and security risk, is China
The only way of industrial sustainable development.Countries in the world scholar has carried out largely the comprehensive utilization of Bayer process red mud for many years
Scientific research produces little effect always.
Citric acid is a kind of stronger organic acid, can be ionized there are three hydrogen ion, and heating can resolve into multi-products,
It reacts with acid, alkali, glycerine etc., calcium salt is more soluble than in hot water in cold water, this property is often identified and isolated from lemon
Acid.Citric acid is easily combined with sodium, generates sodium citrate, sodium citrate not only have non-toxic, regulation performance and it is good surely
It is qualitative, and with extremely strong complexing of metal ion ability.Sodium citrate not only has preferable network to metal ions such as Ca, Mg
Conjunction ability, to other metal ions, there is also good complexing powers.
Invention content
The technical problem to be solved by the present invention is to provide a kind of recycling reuse method of Bayer process red mud, this method tools
There is economical and efficient and convenient for recycling rare metal and the characteristics of constant metal, while also mitigate solid waste bauxite by-product
Harm caused by object red mud bulk deposition.
The present invention adopts the following technical scheme that a kind of recycling of Bayer process red mud recycles to solve above-mentioned technical problem
Method, it is characterised in that the specific steps are：It is sieved after Bayer process red mud is dried, screens out 400-800 hot eyes mud sample product and hydrogen
Sodium oxide molybdena is 1 in mass ratio:0.5-1 is uniformly mixed after 800 DEG C of constant temperature calcining 4h, is taken out sample comminution and is mixed with water
Even, the volume that wherein 1g samples correspond to water is 20-30mL, the heating stirring 1-2h in 100 DEG C of water-bath, is filtered, filtrate adds
It is 10.5 to enter hydrofluoric acid to adjust pH, is uniformly mixed to be placed in kettle of refining and bakes 6-48h in 100 DEG C and obtain zeolite, filter cake
It is dried after repeatedly washing, the mixed acid of the sample after drying and citric acid and acetic acid is added in micro-wave digestion abstraction instrument and is extracted
20-40min is taken to complete the extraction and separation of rare earth element, the sample after wherein 1g drying corresponds to the mixed acid of citric acid and acetic acid
Volume is 20-30mL, and the total mol concentration of citric acid and acetic acid is 1mol/L in the mixed acid of citric acid and acetic acid, citric acid with
The molar ratio of acetic acid is 1:4-4:1.
Further preferably, 1g drying after sample corresponds to citric acid and acetic acid mixed acid volume be 25mL, citric acid
It is 2 with the molar ratio of citric acid and acetic acid in the mixed acid of acetic acid:3, extraction time 30min, rare earth Sc, Y and weight are dilute
Total extraction percentage 76.31% of native Tb, Dy, Ho, Er, Tm, Yb, Lu.
The present invention has the advantages that compared with prior art：
1st, bauxite by-product conventional method is mostly bulk deposition, and landfill pollutes, and the present invention can be effectively using each
Stage product, during heating stirring supernatant can use suitable hydrofluoric acid adjust pH zeolites；
2nd, heteropoly acid is the general name that oxyacid is condensed by prepared by different oxyacid condensations, is the proton of even intensity
By changing molecular composition, acid strength and redox property is adjusted in acid, and have redox ability, in the presence of moisture
The plan liquid phase of formation can also influence its acid and redox property, compared with the inorganic acids extracting process such as hydrochloric acid, citric acid with
The reaction time is shorter under microwave condition and shows better effect of extracting for the mixed acid of acetic acid；
3rd, the content of rare earth extracted from Bayer process red mud sample through extraction processing significantly increases, and improves the profit of mineral resources
With rate, environmental protection while, is also beneficial to the recycling of Bayer process red mud.
Description of the drawings
Fig. 1 is the SEM figures of 400-800 hot eyes mud sample product in the embodiment of the present invention 1；
Fig. 2 is that 400-800 hot eyes mud sample product and sodium hydroxide are 1 in mass ratio in the embodiment of the present invention 1:0.5 roasting sample
The SEM figures of product；
Fig. 3 is the SEM figures of filter cake drying sample after repeatedly washing in the embodiment of the present invention 3；
Fig. 4 is the XRD spectrum of zeolite made from the embodiment of the present invention 2.
Specific embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright range.
Embodiment 1
In the present embodiment, it is sieved after Bayer process red mud is dried, screens out 400-800 hot eyes mud sample product and sodium hydroxide
It is uniformly mixed by different quality proportionings after 800 DEG C of constant temperature calcining 4h, resolution measures rare earth metal total content.
Baking mixed experiment of the table 1 for 400-800 hot eyes mud sample product and sodium hydroxide is cleared up under different proportion value in table
In obtained rare earth total content, quality proportioning 1:0.5 and 1:The sample size that 1 processing method obtains is higher, meets simultaneously
The theory to economize on resources.
The baking mixed experiment of 1 400-800 hot eyes mud sample product of table and sodium hydroxide
Embodiment 2
It is sieved after Bayer process red mud is dried, it is 1 in mass ratio to screen out 400-800 hot eyes mud sample product with sodium hydroxide:
0.5 is uniformly mixed after 800 DEG C of constant temperature calcining 4h, takes out 1g sample comminutions and is uniformly mixed with 20mL water, then at 100 DEG C of water
Heating stirring 1h in bath, filtering, filtrate add in hydrofluoric acid adjust pH be 10.5, be uniformly mixed be placed in kettle of refining in
100 DEG C bake 6h, 12h, for 24 hours and 48h respectively, finally obtain zeolite.
Embodiment 3
Filter cake after filtering after repeatedly washing is dried, the sample after 1.25g drying is weighed respectively and adds in 25mL lemons
The mix acid liquor of acid and acetic acid（The molar concentration of citric acid be respectively 0mol/L, 0.2mol/L, 0.4mol/L, 0.5mol/L,
0.6mol/, 0.8mol/L and 1mol/L, the molar concentration of corresponding acetic acid be respectively 1mol/L, 0.8mol/L, 0.6mol/L,
0.5mol/L, 0.4mol/L, 0.2mol/L and 0mol/L）It shakes up, is put into micro-wave digestion abstraction instrument, at the same pressure, phase
The same time, different mix acid liquors carry out microwave abstracting with sample is compared, according still further to uniform pressure, identical mix acid liquor proportioning, no
Microwave abstracting is carried out to sample with the time.30min, the situation of different mix acid liquor proportionings are extracted in micro-wave digestion abstraction instrument
Under, total extraction percentage of Sc, Y and heavy rare earth Tb, Dy, Ho, Er, Tm, Yb, Lu is respectively 18.16%, 49.38%, 76.31%,
74.26%、71.06%、74.19%、66.04%。
In the mix acid liquor proportioning for being respectively 0.4mol/L and 0.6mol/L in citric acid and acetic acid molar concentration, in microwave
Clear up in abstraction instrument Sc, Y and heavy rare earth Tb, Dy in the case of extraction 10min, 20min, 30min and 40min, Ho, Er, Tm,
Total extraction percentage of Yb, Lu are respectively 20.56%, 49.24%, 76.31%, 64.44%.
Basic principle, main features and advantages embodiment above describes the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. a kind of recycling reuse method of Bayer process red mud, it is characterised in that the specific steps are：Bayer process red mud is dried
After be sieved, it is 1 in mass ratio to screen out 400-800 hot eyes mud sample product and sodium hydroxide:0.5-1 is uniformly mixed after 800 DEG C of perseverances
Temperature roasting 4h, takes out sample comminution and is uniformly mixed with water, and the volume that wherein 1g samples correspond to water is 20-30mL, then at 100 DEG C
Water-bath in heating stirring 1-2h, filtering, filtrate add in hydrofluoric acid adjust pH be 10.5, be uniformly mixed and be placed on kettle of refining
In 6-48h baked in 100 DEG C obtain zeolite, filter cake is dried after repeatedly washing, by the sample after drying and citric acid and acetic acid
Mixed acid be added in micro-wave digestion abstraction instrument extract 30min complete rare earth element extraction and separation, wherein 1g drying after
Sample corresponds to the volume of the mixed acid of citric acid and acetic acid as 25mL, citric acid and acetic acid in the mixed acid of citric acid and acetic acid
Total mol concentration is 1mol/L, and the molar ratio of citric acid and acetic acid is 2:3.
2. the recycling reuse method of Bayer process red mud according to claim 1, it is characterised in that：Rare earth Sc, Y
And 76 .31% of total extraction percentage of heavy rare earth Tb, Dy, Ho, Er, Tm, Yb, Lu.
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| CN201610219802.0A CN105803207B (en) | 2016-04-11 | 2016-04-11 | A kind of recycling reuse method of Bayer process red mud |
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| CN105803207B true CN105803207B (en) | 2018-06-26 |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058995A (en) * | 1990-08-15 | 1992-02-26 | 中国科学院长春应用化学研究所 | Centrifugal extraction process of rare earth ore mother liquor from naphthenic acid |
| CN1844421A (en) * | 2006-03-17 | 2006-10-11 | 汪友华 | Method for extracting scandium from red mud |
| CN102061392A (en) * | 2011-01-27 | 2011-05-18 | 太原理工大学 | Method for extracting scandium from modified red mud by using composite extractant |
| CN102277498A (en) * | 2011-08-08 | 2011-12-14 | 太原理工大学 | Method for enriching rare earth by aluminum oxide red mud |
| CN102994755A (en) * | 2012-09-29 | 2013-03-27 | 贵州绿水青山环保科技有限公司 | Method for recovering ionic rare earth element from red mud |
| CN103215439A (en) * | 2013-04-16 | 2013-07-24 | 内蒙古科技大学 | Method for extracting scandium from scandium enrichment |
| CN103898331A (en) * | 2014-03-28 | 2014-07-02 | 中国铝业股份有限公司 | Method for comprehensive recovery of tantalum and niobium from red mud |
| CN104291540A (en) * | 2014-02-19 | 2015-01-21 | 开封新巨源环保科技开发有限公司 | Resourceful treatment method for red mud |
| CN105331837A (en) * | 2015-12-01 | 2016-02-17 | 中南大学 | Method for gathering scandium from red mud |
-
2016
- 2016-04-11 CN CN201610219802.0A patent/CN105803207B/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058995A (en) * | 1990-08-15 | 1992-02-26 | 中国科学院长春应用化学研究所 | Centrifugal extraction process of rare earth ore mother liquor from naphthenic acid |
| CN1844421A (en) * | 2006-03-17 | 2006-10-11 | 汪友华 | Method for extracting scandium from red mud |
| CN102061392A (en) * | 2011-01-27 | 2011-05-18 | 太原理工大学 | Method for extracting scandium from modified red mud by using composite extractant |
| CN102277498A (en) * | 2011-08-08 | 2011-12-14 | 太原理工大学 | Method for enriching rare earth by aluminum oxide red mud |
| CN102994755A (en) * | 2012-09-29 | 2013-03-27 | 贵州绿水青山环保科技有限公司 | Method for recovering ionic rare earth element from red mud |
| CN103215439A (en) * | 2013-04-16 | 2013-07-24 | 内蒙古科技大学 | Method for extracting scandium from scandium enrichment |
| CN104291540A (en) * | 2014-02-19 | 2015-01-21 | 开封新巨源环保科技开发有限公司 | Resourceful treatment method for red mud |
| CN103898331A (en) * | 2014-03-28 | 2014-07-02 | 中国铝业股份有限公司 | Method for comprehensive recovery of tantalum and niobium from red mud |
| CN105331837A (en) * | 2015-12-01 | 2016-02-17 | 中南大学 | Method for gathering scandium from red mud |
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