CN108751255A - A kind of method and its application of hydrothermal synthesis arsenic natroalunite mixed crystal solid solution - Google Patents
A kind of method and its application of hydrothermal synthesis arsenic natroalunite mixed crystal solid solution Download PDFInfo
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- CN108751255A CN108751255A CN201810672453.7A CN201810672453A CN108751255A CN 108751255 A CN108751255 A CN 108751255A CN 201810672453 A CN201810672453 A CN 201810672453A CN 108751255 A CN108751255 A CN 108751255A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G28/00—Compounds of arsenic
- C01G28/002—Compounds containing, besides arsenic, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of method and its application of hydrothermal synthesis arsenic natroalunite mixed crystal solid solution.Replace synthesis arsenic natroalunite mixed crystal solid solution using the aliovalent isomorph of arsenate and sulfate radical, and be applied to the improvement containing arsenic pollution in trade effluent and mine wastewater, realizes that arsenic in the environment store up by long term stabilization.Basal liquid mainly is prepared using anhydrous sodium sulfate and Patent alum, it is 1 that Na/Al molar ratios, which are made,:Then the arsenic acid solution of different molar concentrations is added in 3 natroalunite presoma, using the arsenic natroalunite mixed crystal solid solution that the aliovalent isomorph of arsenate and sulfate radical substitution synthetic crystallization degree is high, stability is good.This method prepare arsenic natroalunite series of solid solutions compared to conventional hydrothermal synthesis Arsenic fixation method be easily manipulated with material preparation, economic cost is low, can realize arsenic in the environment long term stabilization store up the advantages that.
Description
Technical field
The invention belongs to material security fields, more particularly to a kind of method of hydrothermal synthesis arsenic natroalunite mixed crystal solid solution
And its application.This method utilizes the aliovalent isomorph substitution synthesis arsenic natroalunite series mixed crystal between arsenate and sulfate radical
Solid solution.
Background technology
Arsenic is metalloid, belongs to sulphophile element, there is very strong toxicity and carcinogenicity.Arsenic and its compound are distributed widely in nature
In boundary, the abundance in the earth's crust is 1.7 ~ 1.8 mg/kg, is primarily present in sedimentary rock.Arsenic-containing ores in nature are big absolutely
Majority is pozzuolite compound, and some is mingled in the nonferrous metals ores such as gold, silver, copper, iron, lead, zinc.With industrialized level
It improves, mining, the industrialized levels such as metal smelt and non-ferrous metals processing are promoted, the increase of coal-fired demand, and contain arsenic
The generally use of pigment, active compound and paper, can generate a large amount of arsenic-containing waste water, waste residue and exhaust gas.If these are containing at arsenic pollution
It sets imappropriate, serious environmental pollution can be caused.
Currently, chemical precipitation method because handle arsenic pollution technology maturation and economic cost it is relatively low due to be widely used, utilize
Calcium salt, molysite etc. are co-precipitated to form arsenate compounds hard to tolerate as precipitating reagent and object containing arsenic pollution, reach the mesh of solidification arsenic
's.But a large amount of research shows that using calcium arsenic, iron arsenic is co-precipitated the complicated arsenate compounds to be formed easily by temperature, and pH is even empty
The influence of carbon dioxide in gas can not store up in the environment for a long time.Wherein arsenic acid calcium salt can be with the carbon dioxide exposure in air
Lead to precipitationization so that arsenic release turns again in environment, arsenic acid molysite is vulnerable to temperature and the influence of pH, and arsenic leaches dense
Degree is that 0.5 ~ 82.8 mg/L is differed.Being co-precipitated the complicated arsenate to be formed using calcium salt and molysite and arsenic pollution cannot environment again
Medium-term and long-term stockpiling, there are serious security risks, therefore probe into the pass that can stablize that the precipitating reagent for consolidating arsenic is solution arsenic secondary pollution
Where key.
Alunite group is sulfate mineral, the generally existing in nature, general formula AB3(ZO4)2(OH,H2O)6.Wherein
A can be Na, K, H3The univalent elements such as O can also be Ca, Ba, Pb, the diads such as Bi；B mainly Al and Fe
(Ⅲ)；ZO4Mainly SO4 2-,AsO4 3-And PO4 3-Deng.Same valence or aliovalent class matter can occur for the different points in alunite group
Different types of alunite mineral are generated with as substitution, some researches show that the alunite mineral of generation in different environmental conditions
Under can be stabilized, illustrate that its has the tremendous potential of long-term stockpiling toxic metals.The present invention provides one kind with natroalunite
[NaAl(SO4)2(OH)6] it is basic liquid, replaced using the aliovalent isomorph between arsenate and sulfate radical, is closed using hydro-thermal
At the method for arsenic natroalunite series mixed crystal solid solution, and realize that arsenic in the environment store up by long term stabilization.
Invention content
The object of the present invention is to provide a kind of method and its application of hydrothermal synthesis arsenic natroalunite mixed crystal solid solution.
The thinking of the method for the present invention：Basal liquid is prepared using anhydrous sodium sulfate and Patent alum, obtained Na/Al rubs
You are than being 1:Then 3 natroalunite presoma is added arsenic acid solution, is taken using the aliovalent isomorph of arsenate and sulfate radical
The arsenic natroalunite mixed crystal solid solution high for synthetic crystallization degree, stability is good.
The specific steps are：
(1) 1.8 mol/L metabisulfite solutions of preparation, 5.4 mol/L aluminum sulfate solutions, 1 mol/L arsenic acid solution for standby, wherein
Arsenic acid is prepared by analyzing pure diarsenic pentoxide.
(2) it is 1 by Na/Al molar ratios in container:The metabisulfite solution and aluminum sulfate that 3 addition steps (1) are prepared are molten
Liquid stirs 25 ~ 35 min, and natroalunite basal liquid is made.
(3) 0 ~ 0.3 is pressed:The arsenic acid solution of step (1) preparation is added obtained by step (2) in 1 As/ (As+S) molar ratio
Natroalunite basal liquid in, with 1.00 M H2SO4Or 5.00 M NaOH adjust solution ph to 4.00 ± 0.02, continue to stir
25 ~ 35 min are mixed until being uniformly mixed, mixture are transferred in the closed reactor of polytetrafluoroethylene (PTFE) material liner.
(4) oven temperature is set as 200 DEG C, and the reaction kettle in step (3) is put into the baking oven and reacts 2 h, arsenic sodium is made
Alunite mixed crystal solid solution.
The arsenic natroalunite mixed crystal solid solution of the present invention is applied to realize that arsenic in the environment store up by long term stabilization, specific to walk
Suddenly it is：
Arsenic natroalunite mixed crystal solid solution is naturally cooled into room temperature, is then separated by solid-liquid separation, gained solid phase precipitation object is through super
Pure water 3 ~ 7 times, absolute ethyl alcohol wash 1 ~ 3 time, products therefrom after washing are placed in porcelain dish and is put into baking oven in 105 ~ 110
Dry 24 h, products therefrom are stored up at DEG C, that is, realize that arsenic in the environment store up by long term stabilization.
The present invention is using the high arsenic soda alum of the aliovalent isomorph substitution synthetic crystallization degree between arsenate and sulfate radical
Stone series of solid solutions is easily manipulated compared to conventional hydrothermal synthesis Arsenic fixation method with material preparation, and economic cost is low, can realize
Arsenic in the environment long term stabilization store up the advantages that, for solves the problems, such as consolidate arsenic cause arsenic secondary pollution to provide a kind of new approaches.
Description of the drawings
Fig. 1 is the X-ray diffractogram that the present invention implements arsenic natroalunite mixed crystal solid solution made from 1 ~ 5, PDF 89-3952
For the standard card of natroalunite.
Fig. 2 is the infrared spectrogram that the present invention implements arsenic natroalunite mixed crystal solid solution made from 1 ~ 5.
Fig. 3 is the scanning electron microscope (SEM) photograph that the present invention implements arsenic natroalunite mixed crystal solid solution made from 4.
Specific implementation mode
Embodiment 1：
Under room temperature, 1.8 mol/L metabisulfite solutions and 5.4 mol/L aluminum sulfate solutions, 10 mL is respectively taken to be placed in equipped with 100
In the beaker of mL ultra-pure waters, 35 min are stirred；With 1.00 M H2SO4Or 5.00 M NaOH adjust pH value of solution stablize 4.00 ±
0.02 range；Solution is transferred in the closed reactor of 200 mL polytetrafluoroethylene (PTFE) material liners, is placed in 200 DEG C of baking ovens anti-
2 h are answered, reaction kettle is taken out, arsenic natroalunite mixed crystal solid solution is made.
Arsenic natroalunite mixed crystal solid solution naturally cools to room temperature；Obtained product is separated by solid-liquid separation, solid phase precipitation object warp
Milli-Q water 5 times, absolute ethyl alcohol wash 2 times, and products therefrom after washing is placed in porcelain dish and is put into baking oven and is done at 110 DEG C
Dry 24 h, obtains the natroalunite of high-crystallinity, that is, realizes that arsenic in the environment store up by long term stabilization.
Embodiment 2：
Under room temperature, 1.8mol/L metabisulfite solutions and 5.4 mol/L aluminum sulfate solutions, 10 mL is respectively taken to be placed in equipped with 92.50
In the beaker of mL ultra-pure waters, 35 min are stirred；7.50 mL of arsenic acid solution of 1 mol/L is added in above-mentioned beaker, with 1.00
M H2SO4Or 5.00 M NaOH adjust solution ph and stablize in 4.00 ± 0.02 ranges, continue to stir 35 min；Solution is turned
It moves in the closed reactor of 200 mL polytetrafluoroethylene (PTFE) material liners, is placed in 200 DEG C of baking ovens and reacts 2 h, take out reaction kettle,
The arsenic natroalunite mixed crystal solid solution that As/ (As+S) molar ratio is 0.04 is made.
Arsenic natroalunite mixed crystal solid solution naturally cools to room temperature；Obtained product is separated by solid-liquid separation, solid phase precipitation object warp
Milli-Q water 5 times, absolute ethyl alcohol wash 2 times, products therefrom after washing are placed in porcelain dish and is put into baking oven at 110 DEG C
Dry 24 h, obtain the arsenic natroalunite that As/ (As+S) molar ratio is 0.04, that is, realize arsenic long term stabilization heap in the environment
It deposits.
The above-mentioned arsenic natroalunite mixed crystal solid solution of 4.0 g is weighed respectively to be placed in 3 group of 100 mL polyethylene bottle.And at every group
The HNO of 100 mL initial pH values 2.00 is separately added into bottle3The HNO of solution, initial pH value 4.003Solution and initial pH value 5.60
Ultra-pure water.By this 3 groups of polyethylene bottle sealings, jiggles to be placed in oscillation thermostat water bath and dissolve 180 d, temperature 25 ± 1
℃.Leaching test result is as follows：
PH value dissolves 180 d, 0.013 mmol/L of arsenic leaching concentration under the conditions of being 2.
PH value dissolves 180 d, 0.001 mmol/L of arsenic leaching concentration under the conditions of being 4.
PH value dissolves 180 d, 0.003 mmol/L of arsenic leaching concentration under the conditions of being 5.6.
Embodiment 3：
Under room temperature, 1.8 mol/L metabisulfite solutions and 5.4 mol/L aluminum sulfate solutions, 10 mL is respectively taken to be placed in equipped with 80 mL
In the beaker of ultra-pure water, 35 min are stirred；1 mol/L arsenic acids solution, 20 mL is added in above-mentioned beaker, with 1.00 M H2SO4
Or 5.00 M NaOH adjust solution ph and stablize in 4.00 ± 0.02 ranges, continue to stir 35 min；Solution is transferred to 200
It in the closed reactor of mL polytetrafluoroethylene (PTFE) material liners, is placed in 200 DEG C of baking ovens and reacts 2 h, take out reaction kettle, As/ is made
(As+S) the arsenic natroalunite mixed crystal solid solution that molar ratio is 0.10.
Arsenic natroalunite mixed crystal solid solution naturally cools to room temperature；Obtained product is separated by solid-liquid separation, solid phase precipitation object warp
Milli-Q water 5 times, absolute ethyl alcohol wash 2 times, products therefrom after washing are placed in porcelain dish and is put into baking oven at 110 DEG C
Dry 24 h, obtain the arsenic natroalunite that As/ (As+S) molar ratio is 0.10, that is, realize arsenic long term stabilization heap in the environment
It deposits.
The above-mentioned arsenic natroalunite mixed crystal solid solution of 4.0 g is weighed respectively to be placed in 3 group of 100 mL polyethylene bottle.And at every group
The HNO of 100 mL initial pH values 2.00 is separately added into bottle3The HNO of solution, initial pH value 4.003Solution and initial pH value 5.60
Ultra-pure water.By this 3 groups of polyethylene bottle sealings, jiggles to be placed in oscillation thermostat water bath and dissolve 180 d, temperature 25 ± 1
℃.Leaching test result is as follows：
PH dissolves 180 d, 0.168 mmol/L of arsenic leaching concentration under the conditions of being 2.
PH dissolves 180 d, 0.065 mmol/L of arsenic leaching concentration under the conditions of being 4.
PH dissolves 180 d, 0.066 mmol/L of arsenic leaching concentration under the conditions of being 5.6.
Embodiment 4：
Under room temperature, 1.8 mol/L metabisulfite solutions and 5.4 mol/L aluminum sulfate solutions, 10 mL is respectively taken to be placed in equipped with 55 mL
In the beaker of ultra-pure water, 35 min are stirred；1 mol/L arsenic acids solution, 45 mL is added in above-mentioned beaker, with 1.00 M H2SO4
Or 5.00 M NaOH adjust solution ph and stablize in 4.00 ± 0.02 ranges, continue to stir 35 min；Solution is transferred to 200
It in the closed reactor of mL polytetrafluoroethylene (PTFE) material liners, is placed in 200 DEG C of baking ovens and reacts 2 h, take out reaction kettle, As/ is made
(As+S) the arsenic natroalunite mixed crystal solid solution that molar ratio is 0.20.
Arsenic natroalunite mixed crystal solid solution atural beat is but to room temperature；Obtained product is separated by solid-liquid separation, solid phase precipitation object warp
Milli-Q water 5 times, absolute ethyl alcohol wash 2 times, products therefrom after washing are placed in porcelain dish and is put into baking oven at 110 DEG C
Dry 24 h, obtain the arsenic natroalunite that As/ (As+S) molar ratio is 0.20, that is, realize arsenic long term stabilization heap in the environment
It deposits.
The above-mentioned arsenic natroalunite mixed crystal solid solution of 4.0 g is weighed respectively to be placed in 3 group of 100 mL polyethylene bottle.And at every group
The HNO of 100 mL initial pH values 2.00 is separately added into bottle3The HNO of solution, initial pH value 4.003Solution and initial pH value 5.60
Ultra-pure water.By this 3 groups of polyethylene bottle sealings, jiggles to be placed in oscillation thermostat water bath and dissolve 180 d, temperature 25 ± 1
℃.Leaching test result is as follows：
PH dissolves 180 d, 0.590 mmol/L of arsenic leaching concentration under the conditions of being 2.
PH dissolves 180 d, 0.461 mmol/L of arsenic leaching concentration under the conditions of being 4.
PH dissolves 180 d, 0.461 mmol/L of arsenic leaching concentration under the conditions of being 5.6.
Embodiment 5：
Under room temperature, 1.8 mol/L metabisulfite solutions and 5.4 mol/L aluminum sulfate solutions, 10 mL is respectively taken to be placed in equipped with 43.16
In the beaker of mL ultra-pure waters, 35 min are stirred；It is added in 1 mol/L arsenic acids solution, the 56.84 above-mentioned beakers of mL, with 1.00 M
H2SO4Or 5.00 M NaOH adjust solution ph and stablize in 4.00 ± 0.02 ranges, continue to stir 35 min；Solution is shifted
It into the closed reactor of 200 mL polytetrafluoroethylene (PTFE) material liners, is placed in 200 DEG C of baking ovens and reacts 2 h, take out reaction kettle, system
Obtain the arsenic natroalunite mixed crystal solid solution that As/ (As+S) molar ratio is 0.24.
Arsenic natroalunite mixed crystal solid solution atural beat is but to room temperature；Obtained product is separated by solid-liquid separation, solid phase precipitation object warp
Milli-Q water 5 times, absolute ethyl alcohol wash 2 times, products therefrom after washing are placed in porcelain dish and is put into baking oven at 110 DEG C
Dry 24 h, obtain the arsenic natroalunite that As/ (As+S) molar ratio is 0.24, that is, realize arsenic long term stabilization heap in the environment
It deposits.
The above-mentioned arsenic natroalunite mixed crystal solid solution of 4.0 g is weighed respectively to be placed in 3 group of 100 mL polyethylene bottle.And at every group
The HNO of 100 mL initial pH values 2.00 is separately added into bottle3The HNO of solution, initial pH value 4.003Solution and initial pH value 5.60
Ultra-pure water.By this 3 groups of polyethylene bottle sealings, jiggles to be placed in oscillation thermostat water bath and dissolve 180 d, temperature 25 ± 1
℃.Leaching test result is as follows：
PH dissolves 180 d, 0.558 mmol/L of arsenic leaching concentration under the conditions of being 2.
PH dissolves 180 d, 0.439 mmol/L of arsenic leaching concentration under the conditions of being 4.
PH dissolves 180 d, 0.514 mmol/L of arsenic leaching concentration under the conditions of being 5.6.
Claims (2)
1. a kind of method of hydrothermal synthesis arsenic natroalunite mixed crystal solid solution, it is characterised in that the specific steps are：
(1) 1.8 mol/L metabisulfite solutions of preparation, 5.4 mol/L aluminum sulfate solutions, 1 mol/L arsenic acid solution for standby, wherein
Arsenic acid is prepared by analyzing pure diarsenic pentoxide；
(2) it is 1 by Na/Al molar ratios in container:3 are added the metabisulfite solution and aluminum sulfate solution that step (1) is prepared, and stir
25 ~ 35 min are mixed, natroalunite basal liquid is made；
(3) 0 ~ 0.3 is pressed:Sodium of the arsenic acid solution of step (1) preparation obtained by step (2) is added in 1 As/ (As+S) molar ratio
In alunite basal liquid, with 1.00 M H2SO4Or 5.00 M NaOH adjust solution ph to 4.00 ± 0.02, continue stirring 25 ~
Mixture is transferred to up to being uniformly mixed in the closed reactor of polytetrafluoroethylene (PTFE) material liner by 35 min；
(4) oven temperature is set as 200 DEG C, and the reaction kettle in step (3) is put into the baking oven and reacts 2 h, arsenic soda alum is made
Stone mixed crystal solid solution.
2. a kind of application of method hydrothermal synthesis arsenic natroalunite mixed crystal solid solution as claimed in claim, it is characterised in that the arsenic
Natroalunite mixed crystal solid solution is applied to realize that arsenic in the environment store up by long term stabilization, the specific steps are：
Arsenic natroalunite mixed crystal solid solution is naturally cooled into room temperature, is then separated by solid-liquid separation, gained solid phase precipitation object is through super
Pure water 3 ~ 7 times, absolute ethyl alcohol wash 1 ~ 3 time, products therefrom after washing are placed in porcelain dish and is put into baking oven in 105 ~ 110
Dry 24 h, products therefrom are stored up at DEG C, that is, realize that arsenic in the environment store up by long term stabilization.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110395765A (en) * | 2019-08-18 | 2019-11-01 | 桂林理工大学 | A kind of method of hydrothermal synthesis hidalgoite solid solution |
| CN110407179A (en) * | 2019-08-14 | 2019-11-05 | 中国科学院生态环境研究中心 | A kind of method of synchronous solidification and stabilization arsenic sulfide slag and Sulphur ressource recycling |
| CN110436527A (en) * | 2019-08-18 | 2019-11-12 | 桂林理工大学 | A kind of method of hydrothermal synthesis alkalinity arsenic acid-ferric sulfate solid solution |
| CN110790294A (en) * | 2019-11-22 | 2020-02-14 | 华南理工大学 | NaAl3(SO4)2(OH)6Super-hydrophilic film and preparation method thereof |
| CN112028132A (en) * | 2020-09-13 | 2020-12-04 | 桂林理工大学 | Method for synthesizing arsenopyrite-containing solid solution by precipitation |
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| CN104355374A (en) * | 2014-09-29 | 2015-02-18 | 昆明理工大学 | Sodium arsenic alunite solid solution and preparation method thereof and application of preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407179A (en) * | 2019-08-14 | 2019-11-05 | 中国科学院生态环境研究中心 | A kind of method of synchronous solidification and stabilization arsenic sulfide slag and Sulphur ressource recycling |
| CN110395765A (en) * | 2019-08-18 | 2019-11-01 | 桂林理工大学 | A kind of method of hydrothermal synthesis hidalgoite solid solution |
| CN110436527A (en) * | 2019-08-18 | 2019-11-12 | 桂林理工大学 | A kind of method of hydrothermal synthesis alkalinity arsenic acid-ferric sulfate solid solution |
| CN110790294A (en) * | 2019-11-22 | 2020-02-14 | 华南理工大学 | NaAl3(SO4)2(OH)6Super-hydrophilic film and preparation method thereof |
| CN112028132A (en) * | 2020-09-13 | 2020-12-04 | 桂林理工大学 | Method for synthesizing arsenopyrite-containing solid solution by precipitation |
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