CN104568937A - Determination method for content of metal aluminum in aluminum smelting slag - Google Patents
Determination method for content of metal aluminum in aluminum smelting slag Download PDFInfo
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- CN104568937A CN104568937A CN201510014827.2A CN201510014827A CN104568937A CN 104568937 A CN104568937 A CN 104568937A CN 201510014827 A CN201510014827 A CN 201510014827A CN 104568937 A CN104568937 A CN 104568937A
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Abstract
The invention aims at providing a determination method for the content of metal aluminum in aluminum smelting slag, which can carry out fast analysis on the metal aluminum in the aluminum smelting slag, so as to meet the requirements of analyzing the content of metal aluminum during aluminum smelting slag recycling process. The method comprises the following steps: grinding and screening aluminum smelting slag samples, respectively preparing -100-mesh analytical samples and +100-mesh analytical samples, and adding ferrous sulfate oxidant solution and determining. Based on the analysis technology of metal aluminum in aluminum smelting slag of redox reaction, the method is fast and accurate, the testing demand during aluminum smelting slag recycling process can be realized, the treatment efficiency is high, and social benefits are obvious.
Description
Technical field
The invention belongs to light non-ferrous metal analysis technical field, be specifically related to the assay method of metal aluminum content in a kind of aluminium smelting slag.
Background technology
Along with expanding economy, the consumption of aluminium increases gradually, and bauxite resource becomes in short supply.In primary aluminum, aluminium alloy and secondary aluminium production run, aluminium melt surface can not melt snotter (aluminium smelting slag ash or aluminium smelting slag) by floating one deck, often produce 1 ton of aluminium by generation 30 ~ 50kg aluminium smelting slag, if effectively can not utilize and process this part solid waste, ecologic environment will face serious threat.Aluminium smelting slag composition because of the raw material of each manufacturer and operating conditions different and slightly different, but generally containing aluminium oxide, aluminium nitride, aluminium and other oxide, salt additives etc., it has the inner impurity of Al adsorption melt, suppresses the effect of aluminum oxidation.The oxygen contact reaction of aluminium oxide wherein mainly in aluminum melt and air generates; Aluminium nitride derives from the product that nitrogen in aluminum melt and air or the nitrogen that blasts react; The aluminum melt that aluminium mainly sputters and the aluminum melt that scum silica frost carries out; Other oxide other metal mainly in aluminium alloy is oxidized and produce; Adjuvant mainly contains sodium chloride, potassium chloride and fluoride, mainly plays and reduces flux fusing point, the effect increasing fluidity of molten and prevent aluminum melt to be oxidized.Containing metallic aluminium and alundum (Al2O3) in aluminium ash, in Japan, aluminium ash major part is used to produce aluminium or use as steel-making catalyzer, also has research and utilization aluminium ash to produce fire resistive material.
Different technological processs can produce dissimilar aluminium ash, its Component comparison is complicated, gray is to grey black, 100 mesh sieves can not be crossed completely after grinding, aluminium element content is more than 10%, dominant is four magnesium aluminium oxides, aluminium nitride, aluminium, alundum (Al2O3), silicon dioxide and a small amount of sodium chloride, fluoride, silicon etc. mutually, part aluminium ash has ammonia taste, what wherein most had value is metallic aluminium, Accurate Determining metal aluminum content, for Appropriate application aluminium smelting slag, realize aluminium smelting slag recycling significant.
Summary of the invention
The object of this invention is to provide the assay method of metal aluminum content in a kind of aluminium smelting slag, express-analysis can be carried out to the metallic aluminium in aluminium smelting slag, thus meet the requirement that in aluminium smelting slag recycling process, metal aluminum content is analyzed.
In aluminium smelting slag of the present invention, the assay method of metal aluminum content, comprises the steps:
1) preparation of sample
Sieve after being ground by aluminium smelting slag sample, sieve used is 100 orders (aperture 0.15mm), prepares-100 orders and+100 goal analysis samples respectively; The screening sample that will analyze carry out predrying be placed in exsiccator for subsequent use;
2) analysis of testing sample
Pre-dried-100 orders and+100 objects screening sample being added respectively has in the conical flask of perforated rubber stopper, add calcium carbonate, then iron sulfate oxidizing agent solution is added, to be connected with the perforated rubber stopper of rubber tube beyond the Great Wall rapidly, the outer end clip of rubber tube is clamped to keep in conical flask in anaerobic environment; Conical flask is placed in heating on electric hot plate, keeps slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add phosphoric acid and diphenylamine sulfonic acid sodium solution, then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end;
The contrast blank test not adding sample is done by same step;
3) calculating of testing sample metal aluminum content
By step 2) the volume several generations formula (1) of gained volumetric soiutions:
Al
gold(%)=(V
2-V
1-V
0) × 26.98 × 0.1/3000m × 100 (1)
Wherein, V
2: buret final reading (mL); V
1: buret initial reading (mL); M: testing sample quality (g); V
0: blank solution consumes potassium bichromate solution volume.
Sample metal aluminium content is that-100 orders analyze sample metal aluminium content (Al
-100) analyze sample metal aluminium content (Al with+100 orders
+ 100) weight value, as formula (2)
Al=(Al
-100·m
1+Al
+100·m
2)/(m
1+m
2) (2)。
Wherein the compound method of solution is as follows:
Taking iron sulfate reagent, is iron sulfate by mass volume ratio: sulfuric acid: iron sulfate joins in deionized water by water=200g:75mL:1000mL, preparation iron sulfate oxidizing agent solution;
Taking potassium dichromate reagent, is potassium dichromate by mass volume ratio: potassium dichromate joins in deionized water by water=4.9040g:1000mL, preparation potassium bichromate solution;
Taking diphenylamine sulfonic acid sodium salt, is diphenylamine sulfonic acid sodium salt by mass volume ratio: diphenylamine sulfonic acid sodium salt joins in deionized water by water=0.2g:100mL, preparation diphenylamine sulfonic acid sodium solution.
The invention provides a kind of analytical technology based on metallic aluminium in the aluminium smelting slag of redox reaction, method fast, accurately, can realize the needs checked in aluminium smelting slag recycling process, treatment effeciency of the present invention is high, and social benefit is obvious.
Embodiment
Below by way of instantiation, method of the present invention is described.
Embodiment 1
1) preparation of sample
Muller is utilized to grind 20min under 350r/min by after the division of aluminium smelting slag sample 27006, then 100 mesh sieve are utilized to sieve, prepare-100 orders respectively and analyze sample and+100 orders analysis sample, it is that shared by 86.5% ,+100 orders analysis samples, percentage by weight is 13.5% that-100 orders analyze percentage by weight shared by sample.Analysis sample is carried out at 105 DEG C predrying after, be placed in exsiccator for subsequent use.
2) preparation of solution
Take iron sulfate reagent, by mass volume ratio (iron sulfate: sulfuric acid: water=200g:75mL:1000mL), iron sulfate is joined in deionized water, preparation iron sulfate oxidizing agent solution;
Take potassium dichromate reagent, by mass volume ratio (potassium dichromate: water=4.9040g:1000mL), potassium dichromate is joined in deionized water, preparation potassium bichromate solution;
Take diphenylamine sulfonic acid sodium salt, by mass volume ratio (diphenylamine sulfonic acid sodium salt: water=0.2g:100mL), diphenylamine sulfonic acid sodium salt is joined in deionized water, preparation diphenylamine sulfonic acid sodium solution.
3) analysis of testing sample
Take about 0.1000g-100 order and analyze sample in conical flask, add 20g calcium carbonate, then 100mL iron sulfate oxidizing agent solution is added, to the perforated rubber stopper of rubber tube be connected with beyond the Great Wall rapidly, rubber plug is with holes, hole compact siro spinning technology one rubber tube, the outer end of pipe accompanies a clip, keeps in conical flask in anaerobic environment.Conical flask is placed on electric hot plate in heating, keep slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and with tap water, conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add 10mL phosphoric acid, 3 diphenylamine sulfonic acid sodium solutions, 1 magnet rotor.Then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end.Buret initial reading V
1for 0.15mL, buret final reading V
2for 14.55mL, blank solution consumes iron sulfate volume V
0for 0.00mL, potassium dichromate concentration used is 0.01667mol/L, and calculating-100 orders analysis sample metal aluminium content by formula (1) is 12.3%.
+ 100 orders taking about 0.0500g analyze sample in conical flask, add 20g calcium carbonate, then 100mL iron sulfate oxidizing agent solution is added, to the perforated rubber stopper of rubber tube be connected with beyond the Great Wall rapidly, rubber plug is with holes, hole compact siro spinning technology one rubber tube, the outer end of pipe accompanies a clip, keeps in conical flask in anaerobic environment.Conical flask is placed on electric hot plate in heating, keep slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and with tap water, conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add 10mL phosphoric acid, 3 diphenylamine sulfonic acid sodium solutions, 1 magnet rotor.Then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end, buret initial reading V
1for 0.00mL, buret final reading V
2for 32.11mL, blank solution consumes iron sulfate volume V
0for 0.00mL, potassium dichromate concentration used is 0.01667mol/L, and calculating+100 orders analysis sample metal aluminium content by formula (1) is 56.4%.Be 18.3% by formula (2) weight calculation sample metal aluminum content.
Embodiment 2
1) preparation of sample
Utilize muller to grind 20min under 350r/min by after aluminium smelting slag sample XS001 division, then utilize 100 mesh sieve to sieve, sample is completely by 100 mesh sieve.Analysis sample is carried out at 105 DEG C predrying after, be placed in exsiccator for subsequent use.
2) preparation of solution
Take iron sulfate reagent, by mass volume ratio (iron sulfate: sulfuric acid: water=200g:75mL:1000mL), iron sulfate is joined in deionized water, preparation iron sulfate oxidizing agent solution;
Take potassium dichromate reagent, by mass volume ratio (potassium dichromate: water=4.9040g:1000mL), potassium dichromate is joined in deionized water, preparation potassium bichromate solution;
Take diphenylamine sulfonic acid sodium salt, by mass volume ratio (diphenylamine sulfonic acid sodium salt: water=0.2g:100mL), diphenylamine sulfonic acid sodium salt is joined in deionized water, preparation diphenylamine sulfonic acid sodium solution.
3) analysis of testing sample
Take the analysis sample of about 0.1000g in conical flask, add 20g calcium carbonate, then 100mL iron sulfate oxidizing agent solution is added, to the perforated rubber stopper of rubber tube be connected with beyond the Great Wall rapidly, rubber plug is with holes, hole compact siro spinning technology one rubber tube, the outer end of pipe accompanies a clip, keeps in conical flask in anaerobic environment.Conical flask is placed on electric hot plate in heating, keep slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and with tap water, conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add 10mL phosphoric acid, 3 diphenylamine sulfonic acid sodium solutions, 1 magnet rotor.Then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end.Be 12.2% by calculation sample metal aluminum content.
Embodiment 3
1) preparation of sample
Utilize muller to grind 20min under 350r/min by after aluminium smelting slag sample XS001 division, then utilize 100 mesh sieve to sieve, sample is completely by 100 mesh sieve.Analysis sample is carried out at 105 DEG C predrying after, be placed in exsiccator for subsequent use.
Add 0.0102g, 0.0210g, 0.0321g, 0.0405g, 0.0500g metallic aluminium powder respectively to fill in the conical flask of 0.2000g XS001 analysis sample in 5.
2) preparation of solution
Take iron sulfate reagent, by mass volume ratio (iron sulfate: sulfuric acid: water=200g:75mL:1000mL), iron sulfate is joined in deionized water, preparation iron sulfate oxidizing agent solution;
Take potassium dichromate reagent, by mass volume ratio (potassium dichromate: water=4.9040g:1000mL), potassium dichromate is joined in deionized water, preparation potassium bichromate solution;
Take diphenylamine sulfonic acid sodium salt, by mass volume ratio (diphenylamine sulfonic acid sodium salt: water=0.2g:100mL), diphenylamine sulfonic acid sodium salt is joined in deionized water, preparation diphenylamine sulfonic acid sodium solution.
3) analysis of testing sample
In 5 conical flasks, add 20g calcium carbonate respectively, then add 100mL iron sulfate oxidizing agent solution, will the perforated rubber stopper of rubber tube be connected with beyond the Great Wall rapidly, rubber plug is with holes, hole compact siro spinning technology one rubber tube, the outer end of pipe accompanies a clip, keeps in conical flask in anaerobic environment.Conical flask is placed on electric hot plate in heating, keep slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and with tap water, conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add 10mL phosphoric acid, 3 diphenylamine sulfonic acid sodium solutions, 1 magnet rotor.Then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end.
By calculating, obtain the method recovery as shown in table 1 below.
Table 1: the recovery of the inventive method
Numbering | Add aluminium powder amount/g | Titration volumes/mL | The recovery/% |
1 | 0.0102 | 19.21 | 99.51 |
2 | 0.0210 | 25.16 | 99.31 |
3 | 0.0321 | 31.30 | 99.37 |
4 | 0.0405 | 35.90 | 99.19 |
5 | 0.0500 | 40.92 | 98.40 |
Embodiment 4
1) preparation of sample
Utilize muller to grind 20min under 350r/min by after aluminium smelting slag sample XS003, XS004 division, then utilize 100 mesh sieve to sieve, sample is completely by 100 mesh sieve.Analysis sample is carried out at 105 DEG C predrying after, be placed in exsiccator for subsequent use.
2) preparation of solution
Take iron sulfate reagent, by mass volume ratio (iron sulfate: sulfuric acid: water=200g:75mL:1000mL), iron sulfate is joined in deionized water, preparation iron sulfate oxidizing agent solution;
Take potassium dichromate reagent, by mass volume ratio (potassium dichromate: water=4.9040g:1000mL), potassium dichromate is joined in deionized water, preparation potassium bichromate solution;
Take diphenylamine sulfonic acid sodium salt, by mass volume ratio (diphenylamine sulfonic acid sodium salt: water=0.2g:100mL), diphenylamine sulfonic acid sodium salt is joined in deionized water, preparation diphenylamine sulfonic acid sodium solution.
3) analysis of testing sample
Take 7 parts of about 0.1000gXS003 respectively in conical flask, add 20g calcium carbonate, then 100mL iron sulfate oxidizing agent solution is added, to the perforated rubber stopper of rubber tube be connected with beyond the Great Wall rapidly, rubber plug is with holes, hole compact siro spinning technology one rubber tube, the outer end of pipe accompanies a clip, keeps in conical flask in anaerobic environment.Conical flask is placed on electric hot plate in heating, keep slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and with tap water, conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add 10mL phosphoric acid, 3 diphenylamine sulfonic acid sodium solutions, 1 magnet rotor.Then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end.Analyze the result that sample XS003 records for 7 parts and be respectively 13.66%, 13.67%, 13.70%, 13.62%, 13.58%, 13.49%, 13.61%, 13.62%, the relative standard deviation of test is 0.0693%.
Take about 0.1000g7 part XS004 respectively in conical flask, add 20g calcium carbonate, then 100mL iron sulfate oxidizing agent solution is added, to the perforated rubber stopper of rubber tube be connected with beyond the Great Wall rapidly, rubber plug is with holes, hole compact siro spinning technology one rubber tube, the outer end of pipe accompanies a clip, keeps in conical flask in anaerobic environment.Conical flask is placed on electric hot plate in heating, keep slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and with tap water, conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add 10mL phosphoric acid, 3 diphenylamine sulfonic acid sodium solutions, 1 magnet rotor.Then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end.Analyze the result that sample XS004 records for 7 parts and be respectively 6.27%, 6.36%, 6.30%, 6.23%, 6.29%, 6.30%, 6.31%, 6.29%, the relative standard deviation of test is 0.0393%.
Claims (6)
1. the assay method of metal aluminum content in aluminium smelting slag, it is characterized in that, described method comprises the steps:
1) preparation of sample
Sieve after aluminium smelting slag sample is ground, prepare-100 orders and+100 goal analysis samples respectively; The screening sample that will analyze carry out predrying be placed in exsiccator for subsequent use;
2) analysis of testing sample
Pre-dried-100 orders and+100 objects screening sample being added respectively has in the conical flask of perforated rubber stopper, add calcium carbonate, then iron sulfate oxidizing agent solution is added, to be connected with the perforated rubber stopper of rubber tube beyond the Great Wall rapidly, the outer end clip of rubber tube is clamped to keep in conical flask in anaerobic environment; Conical flask is placed in heating on electric hot plate, keeps slight boiling condition, after question response is complete, take off conical flask, change perforated rubber stopper into atresia rubber plug immediately, and conical flask is cooled, take off rubber plug, with deionized water rinsing bottle wall, add phosphoric acid and diphenylamine sulfonic acid sodium solution, then conical flask is placed on magnetic stirring apparatus, opens stirrer, utilize the solution in potassium bichromate solution titration conical flask, until solution becomes purple be reaction end;
The contrast blank test not adding sample is done by same step;
3) calculating of testing sample metal aluminum content
By step 2) the volume several generations formula (1) of gained volumetric soiutions:
Al
gold(%)=(V
2-V
1-V
0) × 26.98 × 0.1/3000m × 100 (1)
Wherein, V
2: buret final reading (mL); V
1: buret initial reading (mL); M: testing sample quality (g); V
0: blank solution consumes potassium bichromate solution volume;
Sample metal aluminium content is that-100 orders analyze sample metal aluminium content (Al
-100) analyze sample metal aluminium content (Al with+100 orders
+ 100) weight value, as formula (2)
Al=(Al
-100·m
1+Al
+100·m
2)/(m
1+m
2) (2)。
2. the method for claim 1, is characterized in that, described step 1) in screening sieve used be 100 orders, aperture 0.15mm.
3. the method for claim 1, is characterized in that, described step 2) in the addition of calcium carbonate be 200 times that analyze sample quality.
4. the method for claim 1, is characterized in that, described iron sulfate oxidizing agent solution, and its a kind of compound method is as follows:
Take iron sulfate reagent, be iron sulfate by mass volume ratio: sulfuric acid: water=200g:75mL:1000mL, iron sulfate joined in deionized water and completes preparation.
5. the method for claim 1, is characterized in that, described potassium bichromate solution, and its a kind of compound method is as follows:
Take potassium dichromate reagent, be potassium dichromate by mass volume ratio: water=4.9040g:1000mL, potassium dichromate joined in deionized water and has dissolved preparation.
6. the method for claim 1, is characterized in that, described diphenylamine sulfonic acid sodium solution, and its a kind of compound method is as follows:
Take diphenylamine sulfonic acid sodium salt, be diphenylamine sulfonic acid sodium salt by mass volume ratio: water=0.2g:100mL, diphenylamine sulfonic acid sodium salt joined in deionized water and completes preparation.
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