CN104445327B - A kind of method of potassium element in acid treatment aluminium electrolyte - Google Patents
A kind of method of potassium element in acid treatment aluminium electrolyte Download PDFInfo
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- CN104445327B CN104445327B CN201410636296.6A CN201410636296A CN104445327B CN 104445327 B CN104445327 B CN 104445327B CN 201410636296 A CN201410636296 A CN 201410636296A CN 104445327 B CN104445327 B CN 104445327B
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- 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
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/50—Fluorides
- C01F7/54—Double compounds containing both aluminium and alkali metals or alkaline-earth metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/16—Purification
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Abstract
<b>Acid system is removed a method for potassium element in aluminium electrolyte, is characterized in comprising the following steps: (</b><b>1</b><b>) aluminium electrolyte that contains potassium element is joined in concentrated acid solution and reacted, reacted material is filtered, obtain filtrate and filter solid phase, will filter the dry moisture of removing of solid phase, obtain ice crystal; (</b><b>2</b><b>) filtrate is imported in adsorption to K+ molecular sieve and carries out separating of potassium ion and sodium ion, use ammonium nitrate solution to carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization and obtain potassium nitrate; (</b><b>3</b><b>) filtrate after absorption is carried out to evaporative crystallization obtain sodium nitrate. It is high that the present invention is that aluminium electroloysis industry has solved in the Aluminium Electrolysis causing due to the existence of potassium element the degree of superheat, carbon materials is damaged, the series of problems such as electrolytic cell reduction in service life, increase productivity effect, provide practicable method for carry out Aluminum Electrolysis Production under complicated electrolyte system.</b>
Description
Technical field
The present invention relates to the method for potassium sodium cryolite material in a kind of process aluminum electrolytic matter, be specifically related to the method for potassium element in a kind of acid treatment aluminium electrolyte, belong to technical field of inorganic.
Background technology
In recent years, along with developing rapidly of China's Aluminium Industry, the demand of bauxite resource is sharply increased. Therefore a large amount of middle-low bauxites are opened Bian and for the preparation of metallurgical-grade aluminum oxide. In this middle-low bauxite, contain in a large amount of alkali metals, the particularly bauxite of China's bauxite major production areas, sylvite content is higher. The metallurgical-grade aluminum oxide of preparing with this kind of bauxite wherein content of potassium element can be the more than 50 times of external metallurgical-grade aluminum oxide Determination of Potassium. The aluminium oxide that contains in a large number sylvite as raw material for Aluminum Electrolysis Production. This aluminium oxide joins in electrolyte, and sylvite also enters electrolytic cell thereupon together, and constantly in electrolyte, accumulates. Along with continuing of producing, the content of sylvite in electrolyte increases, thereby makes electrolyte component occur to change continuously. Along with the content of potassium in electrolyte progressively raises, electrolyte primary crystal temperature reduces gradually, and under such condition, the degree of superheat can be elevated to more than 30 DEG C sometimes. The degree of superheat is too high, and stove side forms difficulty, and established stove is helped attenuation, affects the stable operation of aluminium cell and the life-span of reducing aluminium cell. And potassium element has very large destruction to the negative electrode of electrolytic cell, this is because the metallic potassium that the potassium ion in fused electrolyte generates at cathode surface infiltrates in cathode material, causes carbon materials is expanded and damaged. Therefore, potassium element has produced very large impact for Aluminium Electrolysis, should adopt afterwards suitable technique to reclaim the potassium element in electrolyte by harmless processing, removes the impact of potassium element for Aluminium Electrolysis. By retrieval analysis, the document that does not have at present potassium sodium cryolite material in process aluminum electrolytic matter is both at home and abroad disclosed report.
Summary of the invention
Object of the present invention is just to solve the problems referred to above that prior art exists, and after research and lot of experiments screen repeatedly, provides the method for potassium element in a kind of acid treatment aluminium electrolyte. The present invention is based on the object of removing harmful element potassium in aluminium electrolyte, successfully work out the technique that this acid treatment contains potassium element aluminium electrolyte, the series of problems such as in the Aluminium Electrolysis causing due to the existence of potassium element, the degree of superheat is high, carbon materials is damaged, electrolytic cell reduction in service life have been solved for aluminium electroloysis industry, both increase productivity effect, provided practicable method for carry out Aluminum Electrolysis Production under complicated electrolyte system again.
The present invention provide technical scheme be.
A method for potassium element in acid treatment aluminium electrolyte, is characterized in comprising the following steps.
(1) by levigate to granularity 100um-150um after the aluminium electrolyte pulverizing that contains potassium element, aluminium electrolyte powder is mixed with technical grade sodium fluoride, join in concentrated acid solution, addition is 75-125g/L according to mixture concentration in concentrated acid solution; Under the condition stirring and heat, react 60-180min, speed of agitator, at 100-300r/min, filters reacted material, obtains reacting rear filtrate and filters solid phase.
(2) filtration solid phase is washed with water to washing lotion aobvious neutral (pH=7.0), the dry moisture of removing, (molecular formula is Na to obtain ice crystal3AlF6）。
(3) filtrate is imported to the adsorbing separation of carrying out potassium ion in the aqueous solution in potassium ion type molecular sieve, carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization and obtain potassium nitrate (molecular formula is KNO3）。
(4) filtrate after absorption being carried out to evaporative crystallization obtains sodium nitrate (molecular formula is NaNO3）。
Concentrated acid solution in described step (1) is HNO3The aqueous solution, concentration 13-65wt%.
Ice crystal purity in described step (2) is more than 95%.
Molecular sieve in described step (3) is potassium ion type absorption molecular sieve, and desorbing agent is 30wt% aqueous ammonium nitrate solution, and potassium nitrate purity is more than 95%.
Sodium nitrate purity in described step (4) is more than 95%.
The aluminium electrolyte powder that contains potassium element and sodium fluoride powder are mixed to join in concentrated acid solution in described step (1), stir and 20 DEG C-100 DEG C at while reacting, should be constant with maintenance cumulative volume to supplementing water in reaction solution.
In the present invention, the dry moisture method of removing for more than drying 1h under 120 ± 5 DEG C of conditions.
Compared with prior art, the invention has the beneficial effects as follows; By the enforcement of technical solution of the present invention, can effectively remove potassium element harmful in electrolyte, can obtain the higher industrial electrolysis matter that is applicable to Aluminum Electrolysis Production of purity simultaneously, can reduce the energy consumption of Aluminum Electrolysis Production; But also can reclaim the industrial chemicals such as potassium nitrate and sodium nitrate, comprehensive average treatment expense is lower, is adapted at carrying out in industrial production application.
The present invention has the following advantages: use and be the common raw material of chemical field, low price, and this scheme of the invention is lower to equipment requirement, common former; Flow process is single, and separable go out many kinds of substance, gained material purity is higher.
The present invention is based on and solve the object of potassium element for the impact of aluminium electroloysis, successfully work out the method for potassium element in acid treatment aluminium electrolyte, affect problem for aluminium electroloysis industry has solved potassium element, also increased benefit, promoted the level of aggregation of China's aluminium electrolytic industry.
Specific embodiments
The aluminium electrolyte sample of processing of the present invention is from certain electrolytic aluminium factory 300kA electrolytic cell, the direct fragmentation of sample, levigate analysis, and this electrolyte contains Na3AlF6、Al2O3、K2NaAlF6; Electrolytical element composition and content Na30.31%, F52.55%, K2.54%, Al13.59%, O1.01%.
The sodium fluoride that wherein the present invention adopts is technical grade sodium fluoride, and composition is containing sodium fluoride >=98% by mass percentage, silica≤0.5, sulfate≤0.3, sodium carbonate≤0.5, water (H2O)≤0.5, other impurity≤0.2%.
In the present invention, the dry moisture method of removing for more than drying 1h under 120 ± 5 DEG C of conditions.
Embodiment 1.
Get 10g aluminium electrolyte, levigate to granularity 100um-150um after pulverizing, obtain aluminium electrolyte powder; Aluminium electrolyte powder is mixed with 2g sodium fluoride powder, and join the HNO of 100ml3In the aqueous solution, HNO3Concentration of aqueous solution is 65wt%; Stir and the condition of 40 DEG C under react 60min, speed of agitator is at 150r/min, constant with maintenance cumulative volume to supplementing water in reaction solution in course of reaction.
Reacted material is filtered, obtain reacting rear filtrate and filter solid phase, filtration solid phase is washed with water to washing lotion aobvious neutral (pH=7.0), the dry moisture of removing, obtaining 10.2g purity is more than 95% ice crystal.
Filtrate is imported and in molecular sieve, carries out separating of potassium ion and sodium ion; Carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization, and to obtain 0.69g purity be 95% above potassium nitrate.
Filtrate after absorption is carried out to evaporative crystallization, and to obtain 3.7g purity be 95% above sodium nitrate.
Embodiment 2.
Get 5g aluminium electrolyte, levigate to granularity 100um-150um after pulverizing, obtain aluminium electrolyte powder; Aluminium electrolyte powder is mixed with 1g sodium fluoride powder, and join the HNO of 50ml3In the aqueous solution, HNO3Concentration of aqueous solution is 65wt%; Stir and the condition of 60 DEG C under react 90min, speed of agitator is at 200r/min, constant with maintenance cumulative volume to supplementing water in reaction solution in course of reaction.
Reacted material is filtered, obtain reacting rear filtrate and filter solid phase, filtration solid phase is washed with water to washing lotion aobvious neutral (pH=7.0), the dry moisture of removing, obtaining 5.11g purity is more than 95% ice crystal.
Filtrate is imported and in molecular sieve, carries out separating of potassium ion and sodium ion; Carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization, and to obtain 0.33g purity be 95% above potassium nitrate.
Filtrate after absorption is carried out to evaporative crystallization, and to obtain 1.75g purity be 95% above sodium nitrate.
Embodiment 3.
Get 150g aluminium electrolyte, levigate to granularity 100um-150um after pulverizing, obtain aluminium electrolyte powder; Aluminium electrolyte powder is mixed with 10g sodium fluoride powder, and join the HNO of 1500ml3In the aqueous solution, HNO3Concentration of aqueous solution is 35wt%; Stir and the condition of 20 DEG C under react 120min, speed of agitator is at 250r/min, constant with maintenance cumulative volume to supplementing water in reaction solution in course of reaction.
Reacted material is filtered, obtain reacting rear filtrate and filter solid phase, filtration solid phase is washed with water to washing lotion aobvious neutral (pH=7.0), the dry moisture of removing, obtaining 152.82g purity is more than 95% ice crystal.
Filtrate is imported and in molecular sieve, carries out separating of potassium ion and sodium ion; Carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization, and to obtain 9.81g purity be 95% above potassium nitrate.
Filtrate after absorption is carried out to evaporative crystallization, and to obtain 12.04g purity be 95% above sodium nitrate.
Embodiment 4.
Get 60g aluminium electrolyte, levigate to granularity 100um-150um after pulverizing, obtain aluminium electrolyte powder; Aluminium electrolyte powder is mixed with 6g sodium fluoride powder, and join the HNO of 800ml3In the aqueous solution, HNO3Concentration of aqueous solution is 22wt%; Stir and the condition of 85 DEG C under react 180min, speed of agitator is at 150r/min, constant with maintenance cumulative volume to supplementing water in reaction solution in course of reaction.
Reacted material is filtered, obtain reacting rear filtrate and filter solid phase, filtration solid phase is washed with water to washing lotion aobvious neutral (pH=7.0), the dry moisture of removing, obtaining 61.14g purity is more than 95% ice crystal.
Filtrate is imported and in molecular sieve, carries out separating of potassium ion and sodium ion; Carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization, and to obtain 3.92g purity be 95% above potassium nitrate.
Filtrate after absorption is carried out to evaporative crystallization, and to obtain 9.35g purity be 95% above sodium nitrate.
Embodiment 5.
Get 500g aluminium electrolyte, levigate to granularity 100um-150um after pulverizing, obtain aluminium electrolyte powder; Aluminium electrolyte powder is mixed with 25g sodium fluoride powder, and join the HNO of 5000ml3In the aqueous solution, HNO3Concentration of aqueous solution is 65wt%; Stir and the condition of 95 DEG C under react 60min, speed of agitator is at 300r/min, constant with maintenance cumulative volume to supplementing water in reaction solution in course of reaction.
Reacted material is filtered, obtain reacting rear filtrate and filter solid phase, filtration solid phase is washed with water to washing lotion aobvious neutral (pH=7.0), the dry moisture of removing, obtaining 509.33g purity is more than 95% ice crystal.
Filtrate is imported and in molecular sieve, carries out separating of potassium ion and sodium ion; Carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization, and to obtain 32.52g purity be 95% above potassium nitrate.
Filtrate after absorption is carried out to evaporative crystallization, and to obtain 23.31g purity be 95% above sodium nitrate.
Claims (6)
1. a method for potassium element in acid treatment aluminium electrolyte, is characterized in that comprising the following steps:
(1) by levigate to granularity 100um-150um after the aluminium electrolyte pulverizing that contains potassium element, aluminium electrolyte powder is mixed with technical grade sodium fluoride, join in concentrated acid solution, addition is 75-125g/L according to mixture concentration in concentrated acid solution; Under the condition stirring and heat, react 60-180min, speed of agitator, at 100-300r/min, filters reacted material, obtains reacting rear filtrate and filters solid phase;
(2) filtration solid phase is washed with water to washing lotion aobvious neutral (pH=7.0), the dry moisture of removing, obtains ice crystal;
(3) filtrate is imported and in potassium ion type molecular sieve, carry out separating of potassium ion and sodium ion; Carry out desorption to adsorbing rear molecular sieve, solution after desorption is carried out to evaporative crystallization and obtain potassium nitrate;
(4) filtrate after absorption is carried out to evaporative crystallization and obtain sodium nitrate.
2. the method for potassium element in a kind of acid treatment aluminium electrolyte according to claim 1, is characterized in that the concentrated acid solution described in step (1) is HNO3The aqueous solution, concentration 13-65wt%.
3. the method for potassium element in a kind of acid treatment aluminium electrolyte according to claim 1, is characterized in that the ice crystal purity described in step (2) is more than 95%.
4. the method for potassium element in a kind of acid treatment aluminium electrolyte according to claim 1, is characterized in that the molecular sieve described in step (3) is potassium ion type absorption molecular sieve, and desorbing agent is 30wt% aqueous ammonium nitrate solution, and potassium nitrate purity is more than 95%.
5. the method for potassium element in a kind of acid treatment aluminium electrolyte according to claim 1, is characterized in that the sodium nitrate purity of telling in step (4) is more than 95%.
6. the method for potassium element in a kind of acid treatment aluminium electrolyte according to claim 1, it is characterized in that the aluminium electrolyte that contains potassium element and sodium fluoride to be mixed to join in concentrated acid solution, stir and 20 DEG C-100 DEG C at while reacting, should be constant with maintenance cumulative volume to supplementing water in reaction solution.
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