CN104340999A - Aluminum oxide purification method - Google Patents
Aluminum oxide purification method Download PDFInfo
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- CN104340999A CN104340999A CN201310401517.7A CN201310401517A CN104340999A CN 104340999 A CN104340999 A CN 104340999A CN 201310401517 A CN201310401517 A CN 201310401517A CN 104340999 A CN104340999 A CN 104340999A
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- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
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Abstract
The invention discloses an aluminum oxide purification method. On the basis of different solubility properties of aluminum oxide and metallic impurity ions thereof in different solvents, metallic ion impurities are selectively dissolved and cleaned through different cleaning solutions, then aluminum oxide is calcined at high temperature of more than 600 DEG C so that metal ion impurities adsorbed in aluminum oxide migrate outside, and the metallic ion impurities are dissolved and cleaned through the cleaning solutions, so as to achieve an effect of separating the metallic impurity ions. The purification method disclosed by the invention has an excellent purification effect on different metallic impurity ions and metallic impurity ions less than 10ppm, and purity of purified aluminum oxide is more than 99.99%, meeting requirement of high-purity aluminum on purity; the adopted cleaning solutions are cheap and recyclable, so that utilization rate of the cleaning solutions is improved, and energy consumption and cost in the purification process are reduced; and the method is simple in process operation, easy to control and excellent in industrial adaptability.
Description
Technical field
The present invention relates to field of aluminum oxide production, especially a kind of method of purification of aluminum oxide.
Background technology
Aluminum oxide is a kind of important industrial chemicals, its moderate purity is called high purity aluminium oxide higher than the aluminum oxide of 99.99%, there are the advantages such as purity is high, specific surface is low, light absorption is high, corrosion-resistant, wear resistance is strong, high temperature resistant, Mohs' hardness is high, good insulating, can be used in the productions such as high-temperature refractory, crucible, porcelain, hard mass, phosphor raw material, high-pressure mercury lamp, special cermacis, YAG laser crystal accessory and surface-mounted integrated circuit.
Aluminum oxide is generally obtained by alkaline process, acid system, using acid and alkali combination method and Re Fa, and the commercial alumina obtained contains other metallic impurity of higher concentration, and purity is generally lower, generally can only reach the purity of 99%.Prior art adopts deionized water, hydrochloric acid, hydrofluoric acid to clean aluminum oxide, to remove some specific metallic impurity.
Realizing in process of the present invention, contriver finds that prior art at least exists following problem:
Prior art only has refining effect to some specific metal ion, and the metal ion of below the 10ppm that cannot purify, the aluminum oxide purity after purification is lower than 99.99%, and cannot reach the purity requirement of rafifinal, refining effect is poor; And prior art processes complicated operation, energy consumption and cost higher.
Summary of the invention
In order to solve prior art to the poor problem of aluminum oxide refining effect, embodiments provide a kind of method of purification of aluminum oxide.Described technical scheme is as follows:
A method of purification for aluminum oxide, said method comprising the steps of:
Step 1: aluminum oxide is placed in reactor, adds scavenging solution, stirs;
Step 2: reactor described in heating steps 1, and be incubated;
Step 3: filter product in described reactor, collects aluminum oxide filter cake, and dry;
Step 4: calcine under the aluminum oxide filter cake of drying is placed in the temperature of more than 600 DEG C;
Step 5: the aluminum oxide after calcining is placed in reactor, adds scavenging solution, stir;
Step 6: reactor described in heating steps 5, and be incubated;
Step 7: product in filtration reactor, collects aluminum oxide filter cake, and dry.
Particularly, in described step 3 and described step 7: also comprise with scavenging solution repeated washing aluminum oxide filter cake 1-8 time.
In described step 2 and described step 6: 25 DEG C-85 DEG C are heated to described reactor, insulation 10min-6h.
In described step 4: the temperature of calcining aluminum oxide is 600 DEG C-2000 DEG C.
As preferably, in described step 4: carrying out calcining temperature to aluminum oxide is 1300 DEG C-1800 DEG C.
Particularly, in described step 1 and described step 5: the quality of aluminum oxide and scavenging solution is 1:1 ~ 1:20 than scope;
At least one in the salts solution that described scavenging solution comprises deionized water, inorganic acid solution, organic acid soln, organic basic solution, positively charged ion are nonmetallic ion, aromatic hydrocarbon.
At least one in oxygenant, reductive agent, complexing agent is also comprised in described scavenging solution.
Particularly, described reactor is any one in 316L stainless steel reactor, PE reactor, PP reactor, tetrafluoroethylene reactor, enamel reactor, 316L stainless steel lined PE reactor, 316L stainless steel lined PP reactor, 316L stainless steel lined tetrafluoroethylene reactor.
Particularly, as preferably, described reactor is tetrafluoroethylene reactor.
The dissolving properties that the method for the invention utilizes aluminum oxide different in different solvents from its metallic impurity ion, optionally impurity metal ion dissolved by different scavenging solutions and clean, in conjunction with more than 600 DEG C high-temperature calcination aluminum oxide, the impurity metal ion being adsorbed on aluminum oxide inside is moved outside again, by scavenging solution impurity metal ion dissolved again and clean, thus reaching the effect being separated and removing metallic impurity ion.
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is:
The embodiment of the present invention adopts dissimilar scavenging solution to clean the mode combined with more than 600 DEG C high-temperature calcinations, by changing alumina crystal structure, the metallic impurity ion being adsorbed on aluminum oxide inside is moved outside, and cleans with scavenging solution, reach the object of alumina purifying.Have the stronger selection property removed to dissimilar metallic impurity ion, also have good removal effect to the metallic impurity ion of below 10ppm, the aluminum oxide purity after purification, higher than 99.99%, reaches the purification requirement of rafifinal; Scavenging solution used is cheap, reusable, improves the utilization ratio of scavenging solution, reduces energy consumption and the cost of purification process; And embodiment of the present invention technological operation is comparatively simple, easy to control, there is good industrialization adaptability.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the process flow sheet of the method for purification of a kind of aluminum oxide that the embodiment of the present invention provides.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing 1, embodiment of the present invention is described further in detail.
Embodiment one
Embodiments provide a kind of method of purification of aluminum oxide, comprise the following steps:
Step 1: aluminum oxide is placed in reactor, adds scavenging solution, stirs;
Step 2: reactor described in heating steps 1, and be incubated;
Step 3: filter product in described reactor, collects aluminum oxide filter cake, and dry;
Step 4: calcine under the aluminum oxide filter cake of drying is placed in the temperature of more than 600 DEG C;
Step 5: the aluminum oxide after calcining is placed in reactor, adds scavenging solution, stir;
Step 6: reactor described in heating steps 5, and be incubated;
Step 7: product in filtration reactor, collects aluminum oxide filter cake, and dry.
In the embodiment of the present invention, impurity metal ion often exists with the form of oxide compound or other compounds, based on this, the present invention utilizes following three modes to remove impurity metal ion: first kind of way: dissolve after reaction, the compound of some metal ion is insoluble in deionized water or organic solvent, but with acid, alkali, after salt reacts, namely deionized water or organic solvent is dissolvable in water, therefore the metal ion of this class can by adding acid by aluminum oxide, alkali, in the aqueous solution of salt or organic solution, metal ion and acid, alkali, reactant salt dissolves, and aluminum oxide does not react with it, thus reach refining effect.The second way: dissolve after complexing, even if the compound of some metal ion also cannot react dissolving at the solution of acid, alkali, salt, now can, by adding complexing agent, by these complexing of metal ion, thus it be made to be dissolved in deionized water or organic solvent.The third mode: the arrangement of some alumina crystal structure is uneven, and aluminum ion is irregular to be distributed in crystal, easily cause the electronegative situation in local to produce, other ionic impurities are easily adsorbed in compound; Some aluminum oxide internal surface area is large, there is vesicular structure, easily allows other ionic impurities adsorb.By carrying out high-temperature calcination to aluminum oxide, alumina crystal structure changes, originally aluminum ion pockety is evenly distributed in crystal, no longer there is partial-band negative electricity causes other metal ions to be easily adsorbed in aluminum oxide, and simultaneous oxidation aluminum ratio surface-area diminishes, and vesicular structure changes, originally other ionic impurities being adsorbed on internal surface are moved outside, spend scavenging solution again to clean, just can remove foreign metal ion, thus reach the effect of alumina purifying.
In step 2 described in the embodiment of the present invention and described step 6: 25 DEG C-85 DEG C are heated to described reactor, insulation 10min-6h, temperature is too low, and can cause reaction, dissolve slow, speed of reaction reduces, and reduces the efficiency of purification; Temperature is too high, scavenging solution can be caused to volatilize, decompose seriously, cause inefficacy and the waste of scavenging solution.Increase the energy consumption and cost of purifying, reduce the efficiency of purifying.
In the embodiment of the present invention, described step 3 and described step 7 also comprise: use scavenging solution repeated washing aluminum oxide filter cake 1-8 time.Aluminum oxide filter cake cleans once in the reactor, according to purification needs, in filter plant or in reactor, scavenging solution directly rinses, and carry out repeatedly repeated washing to filter cake, scavenging solution is reusable, improve the utilization ratio of scavenging solution, reduce the energy consumption and cost of purifying.
The mode of filtering described in described step 3 and described step 7 adopts at least one in natural filtration, press filtration, centrifugation.
In the embodiment of the present invention, in described step 4: the temperature of calcining aluminum oxide is 600 DEG C-2000 DEG C.As preferably, the temperature of calcining aluminum oxide is 1300 DEG C-1800 DEG C.
Calcining temperature effectively will could change alumina crystal structure more than 600 DEG C, calcining temperature is higher, and the uniformity coefficient that aluminum ion is reset is higher, and metallic impurity ion more easily moves outside, the refining effect of aluminum oxide is more obvious, and embodiment of the present invention preferable temperature is 1300 DEG C-1800 DEG C.
In the embodiment of the present invention, in described step 1 and described step 5: the quality of aluminum oxide and scavenging solution is 1:1 ~ 1:20 than scope; At least one in the salts solution that described scavenging solution comprises deionized water, inorganic acid solution, organic acid soln, organic basic solution, positively charged ion are nonmetallic ion, aromatic hydrocarbon.At least one in oxygenant, reductive agent, complexing agent is also comprised in described scavenging solution.
The different scavenging solutions selected in the embodiment of the present invention have obvious selective purification effect to different metallic elements.Impurity metal ion mainly exists with the form of the oxide compound of the elements such as Fe, Na, K, Ca, Mg, Cu, Zn, Ni or compound.Wherein the salts solution of pure water scavenging solution, nonmetallic ion and aromatic hydrocarbon have good solubility property to Na, K element, can reduce the content of Na in aluminum oxide, K element greatly; Acidic cleaning solution have good selectivity to Fe, Mg, Ca unit, can react and dissolve more Fe, Mg, Ca impurity; Alkaline cleaning fluid have good selectivity to Zn unit, can promote the dissolving of Zn element, and such as, the alkaline cleaning fluids such as ammoniacal liquor can form complex compound with Zn, promotes to dissolve.
In order to prevent from existing in the lattice of metallic impurity compound the residual of unreacted elemental metals, oxygenant can be added these elemental metals are oxidized into oxide compound are then dissolved in scavenging solution in scavenging solution, thus improving the refining effect of aluminum oxide.In addition, iron protoxide, Z 250 can also be oxidized into ferric oxide by oxygenant, make it more easily and scavenging solution reacts, thus are dissolved in scavenging solution.
The scavenging solution special to some and ion can use reductive agent, such as when using alkaline cleaning fluid, add reductive agent, ironic hydroxide reduction can be become the higher ferrous hydroxide of solubleness, ferrous hydroxide can react with alkali and generate the higher hexahydroxy-of solubleness and close ferrous ion, and be dissolved in scavenging solution, more effectively remove Fe element impurity.
Complexing agent can form stable water soluble complex with many metal ions, and these metal ions are more easily taken away by scavenging solution.
Reactor described in the embodiment of the present invention is any one in 316L stainless steel reactor, PE reactor, PP reactor, tetrafluoroethylene reactor, enamel reactor, 316L stainless steel lined PE reactor, 316L stainless steel lined PP reactor, 316L stainless steel lined tetrafluoroethylene reactor.The material of described reactor can not react to introduce impurity with cleaning liquid, so the reactor of preferably polytetrafluoroethylene material.
The method of purification of a kind of aluminum oxide that the embodiment of the present invention provides also can be used for Tai-Ace S 150 and aluminium hydroxide to purify, and after purifying, Tai-Ace S 150 and aluminium hydroxide directly can prepare the aluminum oxide of higher degree.
The method of a kind of alumina purifying that the embodiment of the present invention provides, dissimilar scavenging solution is adopted to clean the mode combined with more than 600 DEG C high-temperature calcinations, by changing alumina crystal structure, the metallic impurity ion being adsorbed on aluminum oxide inside is moved outside, and clean with scavenging solution, reach the object of alumina purifying.Have the stronger selection property removed to dissimilar metallic impurity ion, also have good removal effect to the metallic impurity ion of below 10ppm, the aluminum oxide purity after purification, higher than 99.99%, reaches the purification requirement of rafifinal; Scavenging solution used is cheap, reusable, improves the utilization ratio of scavenging solution, reduces energy consumption and the cost of purification process; Technological operation is simple, easy to control, has good industrialization adaptability.
Embodiment two
150 grams of elementary metal impurities content are put into the tetrafluoroethylene of 2L higher than the aluminum oxide of 60ppm, add 1% ammoniacal liquor 1500 grams, open and stir, be heated to 60 DEG C of insulation 3h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the filtration cakes torrefaction finally obtained, obtain the aluminum oxide of 148 grams of metallic impurity higher than 40ppm.
Metallic impurity ion content contrast table in the different aluminum oxide of table 1
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 18.77 | 15.65 |
| Magnesium | 2.357 | 2.460 |
| Calcium | 15.46 | 8.879 |
| Copper | 0.487 | 0.579 |
| Cobalt | 0.658 | 0.665 |
| Nickel | 0.613 | 0.578 |
| Sodium | 3.784 | 1.987 |
| Potassium | 4.985 | 2.985 |
| Zinc | 19.685 | 14.858 |
| Add up to | 66.799 | 48.641 |
The embodiment of the present invention adopts the ammonia soln of 1% repeatedly to clean aluminum oxide as scavenging solution, table 1 shows, less part metals foreign ion and scavenging solution is only had to carry out reacting and dissolving, major part metallic impurity ion is not removed, the removal of impurity of product is only about 27.18%, and metallic impurity ion remaval effect is poor.
Embodiment three
150 grams of elementary metal impurities content are calcined 3h higher than the aluminum oxide of 70ppm at 1300 DEG C and obtains the aluminum oxide of elementary metal impurities content higher than 70ppm.
Metallic impurity ion content contrast table in the different aluminum oxide of table 2
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 17.65 | 17.13 |
| Magnesium | 3.587 | 3.240 |
| Calcium | 18.958 | 17.958 |
| Copper | 1.465 | 1.545 |
| Cobalt | 0.897 | 0.902 |
| Nickel | 0.578 | 0.588 |
| Sodium | 8.987 | 9.054 |
| Potassium | 3.878 | 4.285 |
| Zinc | 17.658 | 16.787 |
| Add up to | 73.658 | 71.489 |
The embodiment of the present invention adopts the mode of 1300 DEG C of high-temperature calcination 3h to purify to aluminum oxide, and as shown in Table 2, metallic impurity ion is not removed substantially, and the removal of impurity of product is only 0.03%, the non-constant of metallic impurity ion remaval effect.
Embodiment four
150 grams of elementary metal impurities content are put into the 316L stainless steel reactor of 2L higher than the aluminum oxide of 200ppm, add deionized water 1500 grams, open and stir, be heated to 80 DEG C of insulation 2h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the filtration cakes torrefaction finally obtained, 4h is calcined at 1300 DEG C, take out the 316L stainless steel reactor that product puts into 2L, add deionized water 1500 grams, open and stir, be heated to 80 DEG C of insulation 2h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the aluminum oxide of 148 grams of elementary metal impurities content lower than 20ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 3
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 3.794 | 2.537 |
| Magnesium | 1.424 | 0.815 |
| Calcium | 9.43 | 1.01 |
| Copper | 0.395 | 0.165 |
| Cobalt | 0.744 | 0.45 |
| Nickel | 0.1 | 0.1 |
| Sodium | 155.6 | 5.993 |
| Potassium | 33.82 | 1.543 |
| Zinc | 6.234 | 3.504 |
| Add up to | 211.541 | 16.117 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1300 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 3, metallic impurity ion removes in a large number, the removal of impurity of product is up to 92.4%, aluminum oxide high purity 99.998% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment five
150 grams of elementary metal impurities content are put into the PE reactor of 4L higher than the aluminum oxide of 50ppm, add deionized water 3000 grams, open and stir, be heated to 25 DEG C of insulation 6h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the filtration cakes torrefaction finally obtained, 3.5h is calcined at 1800 DEG C, take out the PE reactor that product puts into 4L, add deionized water 3000 grams, open and stir, be heated to 25 DEG C of insulation 6h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the aluminum oxide of 148 grams of elementary metal impurities content lower than 10ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 4
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 2.662 | 2.477 |
| Magnesium | 0.949 | 0.726 |
| Calcium | 2.482 | 0.685 |
| Copper | 0.859 | 0.237 |
| Cobalt | 1.846 | 0.276 |
| Nickel | 0.05 | 0 |
| Sodium | 22.05 | 1.038 |
| Potassium | 24.57 | 0.337 |
| Zinc | 2.335 | 2.716 |
| Add up to | 57.803 | 8.492 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1800 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 4, metallic impurity ion removes in a large number, the removal of impurity of product is up to 85.31%, aluminum oxide high purity 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment six
150 grams of elementary metal impurities content are put into the PP reactor of 2L higher than the aluminum oxide of 50ppm, add deionized water 150 grams, open and stir, be heated to 55 DEG C of insulation 10min, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 5 times, the filtration cakes torrefaction finally obtained, 3h is calcined at 600 DEG C, take out the PP reactor that product puts into 2L, add deionized water 150 grams, open and stir, be heated to 55 DEG C of insulation 10min, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, obtain the aluminum oxide of 148 grams of elementary metal impurities content lower than 20ppm.
Metallic impurity ion content contrast table in the different aluminum oxide of table 5
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 2.779 | 2.221 |
| Magnesium | 1.549 | 0.599 |
| Calcium | 7.739 | 2.54 |
| Copper | 0.309 | 0.309 |
| Cobalt | 0.352 | 0.476 |
| Nickel | 0 | 0 |
| Sodium | 23.18 | 4.375 |
| Potassium | 20.33 | 3.25 |
| Zinc | 2.724 | 2.874 |
| Add up to | 58.962 | 16.644 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-600 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 5, the removal of impurity of product is up to 72%, and the aluminum oxide high purity 99.998% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment seven
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminum oxide of 60ppm, add 1% hydrochloric acid soln 1500 grams, open and stir, be heated to 85 DEG C of insulation 80min, solution is filtered, by the filtration cakes torrefaction obtained, 4h is calcined at 1500 DEG C, take out the tetrafluoroethylene reactor that product puts into 2L, add 1% hydrochloric acid soln 1500 grams, open and stir, be heated to 85 DEG C of insulation 80min, solution is filtered, after drying, obtains the aluminum oxide of 148 grams of elementary metal impurities content lower than 10ppm.
Metallic impurity ion content contrast table in the different aluminum oxide of table 6
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 21.76 | 1.162 |
| Magnesium | 2.487 | 0.564 |
| Calcium | 28.07 | 1.817 |
| Copper | 0.116 | 0.146 |
| Cobalt | 0.147 | 0.179 |
| Nickel | 0.459 | 0 |
| Sodium | 202.846 | 3.85 |
| Potassium | 101.584 | 4.359 |
| Zinc | 5.872 | 2.917 |
| Add up to | 363.341 | 14.994 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1500 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 6, the removal of impurity of product is up to 98.87%, and the aluminum oxide high purity 99.998% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment eight
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminum oxide of 70ppm, add 1% oxalic acid solution 1500 grams, open and stir, be heated to 60 DEG C of insulation 1h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 8 times, the filtration cakes torrefaction finally obtained, 3h is calcined at 1300 DEG C, take out the tetrafluoroethylene reactor that product puts into 2L, add 1% oxalic acid solution 1500 grams, open and stir, be heated to 60 DEG C of insulation 1h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the aluminum oxide of 148 grams of elementary metal impurities content lower than 10ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 7
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 28.52 | 1.501 |
| Magnesium | 1.734 | 0.49 |
| Calcium | 26.6 | 1.407 |
| Copper | 0.466 | 0.083 |
| Cobalt | 0.539 | 0.24 |
| Nickel | 0 | 0 |
| Sodium | 15.36 | 2.071 |
| Potassium | 0.699 | 0.445 |
| Zinc | 2.306 | 2.56 |
| Add up to | 76.224 | 8.797 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1300 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 7, the removal of impurity of product is up to 88.50%, and the aluminum oxide high purity 99.999% after purification, reaches the purity requirement of rafifinal.Also can be found out by table 7, select oxalic acid solution to be scavenging solution, to iron, the removal effect of the element such as magnesium and calcium is fairly obvious, and selectivity is strong.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment nine
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminum oxide of 50ppm, add 1% ammonia soln 1500 grams, open and stir, be heated to 70 DEG C of insulation 2.5h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 2 times, the filtration cakes torrefaction finally obtained, 3.5h is calcined at 1800 DEG C, put into the tetrafluoroethylene reactor of 2L, add 1% ammonia soln 1500 grams, open and stir, be heated to 70 DEG C of insulation 2.5h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the aluminum oxide of 148 grams of elementary metal impurities content lower than 20ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 8
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 13.58 | 7.008 |
| Magnesium | 1.712 | 0.567 |
| Calcium | 25.1 | 0.545 |
| Copper | 0.188 | 0.133 |
| Cobalt | 0.59 | 0.311 |
| Nickel | 0 | 0 |
| Sodium | 2.706 | 1.503 |
| Potassium | 1.371 | 0.073 |
| Zinc | 6.961 | 0.898 |
| Add up to | 52.208 | 11.038 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1800 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 8, the removal of impurity of product is up to 80%, and the aluminum oxide high purity 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment ten
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminum oxide of 50ppm, add 1% oxalic acid solution 1500 grams, open and stir, be heated to 60 DEG C of insulation 3h, solution is filtered, the filter cake obtained is reentered in the tetrafluoroethylene reactor of 2L, add 1% ammonia soln 1500 grams, open and stir, be heated to 50 DEG C of insulation 3h, solution is filtered and obtains filter cake, 5h is calcined at 2000 DEG C, take out the tetrafluoroethylene reactor that product puts into 2L, add deionized water 1500 grams, open and stir, be heated to 60 DEG C of insulation 3h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 5 times, the aluminum oxide of 142 grams of elementary metal impurities content lower than 10ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 9
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 16.06 | 1.359 |
| Magnesium | 1.594 | 0.596 |
| Calcium | 27.56 | 0.133 |
| Copper | 0.121 | 0.124 |
| Cobalt | 0.227 | 0.611 |
| Nickel | 0.199 | 0 |
| Sodium | 2.739 | 1.618 |
| Potassium | 0.841 | 0.033 |
| Zinc | 7.48 | 1.638 |
| Add up to | 56.821 | 6.112 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-2000 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 9, the removal of impurity of product is up to 90%, and the aluminum oxide high purity more than 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment 11
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminum oxide of 30ppm, add 1% ammonium fluoride solution 1500 grams, open and stir, be heated to 75 DEG C of insulation 1.5h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 6 times, the filtration cakes torrefaction finally obtained, calcine 3 hours at 1600 DEG C, take out the tetrafluoroethylene reactor that product puts into 2L, add deionized water 1500 grams, open and stir, be heated to 75 DEG C of insulation 1.5h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the aluminum oxide of 148 grams of elementary metal impurities content lower than 20ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 10
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 2.18 | 1.313 |
| Magnesium | 1.351 | 0.518 |
| Calcium | 22.07 | 0.354 |
| Copper | 0.094 | 0.039 |
| Cobalt | 0.479 | 0.25 |
| Nickel | 0 | 0 |
| Sodium | 2.675 | 2.576 |
| Potassium | 1.203 | 0.542 |
| Zinc | 2.692 | 2.227 |
| Add up to | 32.744 | 7.819 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1600 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, and as seen from Table 10, the aluminum oxide high purity more than 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment 12
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminum oxide of 70ppm, add 1% salpeter solution 1500 grams, add 10 grams, complexing agent tartrate.Open and stir, be heated to 60 DEG C of insulation 3h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the filtration cakes torrefaction finally obtained, calcines 3h at 1650 DEG C, takes out the tetrafluoroethylene reactor that product puts into 2L, add 1% salpeter solution 1500 grams, add 10 grams, complexing agent tartrate.Open and stir, be heated to 60 DEG C of insulation 3h, solution filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, after drying, obtains the aluminum oxide of 145 grams of elementary metal impurities content lower than 10ppm.
Metallic impurity ion content contrast table in the different aluminum oxide of table 11
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 15.09 | 0.922 |
| Magnesium | 2.329 | 0.436 |
| Calcium | 24.67 | 0.291 |
| Copper | 0.095 | 0.103 |
| Cobalt | 0.482 | 0.384 |
| Nickel | 0 | 0 |
| Sodium | 3.855 | 1.526 |
| Potassium | 1.601 | 0.387 |
| Zinc | 2.339 | 2.347 |
| Add up to | 50.461 | 6.396 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1650 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, and as seen from Table 11, the aluminum oxide high purity more than 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment 13
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminum oxide of 70ppm, add 1% ammoniacal liquor 1500 grams, add complexing agent trolamine 10 grams.Open and stir, be heated to 65 DEG C of insulation 3.5h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 1 time, the filtration cakes torrefaction finally obtained, calcines 2.7h at 1700 DEG C, takes out the tetrafluoroethylene reactor that product puts into 2L, add 1% ammoniacal liquor 1500 grams, add complexing agent trolamine 10 grams.Open and stir, be heated to 65 DEG C of insulation 3.5h, solution filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, after drying, obtains the aluminum oxide of 145 grams of elementary metal impurities content lower than 10ppm.
Metallic impurity ion content contrast table in the different aluminum oxide of table 12
| Test event | Raw alumina (ppm) | Purification rear oxidation aluminium (ppm) |
| Iron | 11.65 | 0.987 |
| Magnesium | 2.288 | 0.507 |
| Calcium | 18.21 | 0.526 |
| Copper | 0.595 | 0.124 |
| Cobalt | 0.529 | 0.265 |
| Nickel | 0.605 | 0.5 |
| Sodium | 4.99 | 1.523 |
| Potassium | 4.915 | 0.132 |
| Zinc | 18.057 | 0.794 |
| Add up to | 61.839 | 5.358 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1700 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, as seen from Table 12, the removal of impurity of product is up to 92%, and the aluminum oxide high purity more than 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment 14
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the Tai-Ace S 150 of 20ppm, add toluene 1500 grams, open and stir, be heated to 60 DEG C of insulation 1h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the filtration cakes torrefaction finally obtained, put into retort furnace again at 1000 DEG C of calcining 3h, take out the tetrafluoroethylene reactor that product puts into 2L, add toluene 1500 grams, open and stir, be heated to 60 DEG C of insulation 1h, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the Tai-Ace S 150 of 148 grams of elementary metal impurities content lower than 10ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 13
| Test event | Raw material sulphuric acid aluminium | Tai-Ace S 150 after purifying |
| Iron | 2.771 | 2.557 |
| Magnesium | 0.874 | 0.392 |
| Calcium | 14.23 | 1.201 |
| Copper | 0.172 | 0.071 |
| Cobalt | 0.464 | 0.505 |
| Nickel | 0.174 | 0 |
| Sodium | 2.772 | 1.023 |
| Potassium | 0.523 | 0.225 |
| Zinc | 2.75 | 1.268 |
| Add up to | 24.73 | 7.242 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1000 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, and as seen from Table 13, the aluminum oxide high purity more than 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
Embodiment 15
150 grams of elementary metal impurities content are put into the tetrafluoroethylene reactor of 2L higher than the aluminium hydroxide of 50ppm, add 1500 grams, the nitric acid of 1%, open and stir, be heated to 65 DEG C of insulation 70min, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the filtration cakes torrefaction finally obtained, 3h is calcined at 1500 DEG C, take out the tetrafluoroethylene reactor that product puts into 2L, add 1500 grams, the nitric acid of 1%, open and stir, be heated to 65 DEG C of insulation 70min, solution is filtered, the filter cake obtained is repeated above-mentioned cleaning operation 4 times, the aluminum oxide of 148 grams of elementary metal impurities content lower than 10ppm is obtained after drying.
Metallic impurity ion content contrast table in the different aluminum oxide of table 14
| Test event | Raw aluminum hydroxide | Purification rear oxidation aluminium |
| Iron | 13.56 | 1.038 |
| Magnesium | 0.552 | 0.224 |
| Calcium | 18.77 | 1.054 |
| Copper | 0.151 | 0.077 |
| Cobalt | 0.502 | 0.484 |
| Nickel | 0.133 | 0 |
| Sodium | 15.28 | 0.775 |
| Potassium | 3.651 | 0.232 |
| Zinc | 2.550 | 1.560 |
| Add up to | 55.149 | 5.444 |
The embodiment of the present invention adopts the mode of scavenging solution cleaning-1500 DEG C of high-temperature calcinations-scavenging solution cleaning to purify to aluminum oxide, and as seen from Table 14, the aluminum oxide high purity more than 99.999% after purification, reaches the purity requirement of rafifinal.
Embodiment of the present invention tool has the following advantages: product purity is high, applied widely; Selectivity is strong, is applicable to some and controls very strict product to individual event metal ion; Production technique is simple, convenient; No coupling product, environmentally safe; Purify required with low cost.
In above embodiment: embodiment two and embodiment three are comparative example, this comparative example and above all embodiments contrast can find out that aluminum oxide must calcining simultaneously through 1, more than more than 600 DEG C, 2, scavenging solution is used to clean two operations, just can reach refining effect, lack wherein any one and all cannot reach purification requirement.Alumina product can be purified to purity higher than more than 99.99% by the method for purification of the embodiment of the present invention, reaches the purity requirement of rafifinal.Refining effect can being found out, different scavenging solutions has obvious selective purification effect to different metallic elements, and wherein pure water scavenging solution has good refining effect to Na, K element; Acidic cleaning solution have good refining effect to Fe, Mg, Ca unit; Alkaline cleaning fluid have good refining effect to Zn unit;
In the embodiment of the present invention, in aluminum oxide, elementary metal impurities content all adopts PerkinElmer company Optima7000DV series ICP-OES(Inductively coupled plasma optical emission spectrometer) experiment Analysis, constituent content all adopts uniform units: ppm(parts per million), namely represent 1,000,000/(several).
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a method of purification for aluminum oxide, is characterized in that, described method of purification comprises the following steps:
Step 1: aluminum oxide is placed in reactor, adds scavenging solution, stirs;
Step 2: reactor described in heating steps 1, and be incubated;
Step 3: filter product in described reactor, collects aluminum oxide filter cake, and dry;
Step 4: calcine under the aluminum oxide filter cake of drying is placed in the temperature of more than 600 DEG C;
Step 5: the aluminum oxide after calcining is placed in reactor, adds scavenging solution, stir;
Step 6: reactor described in heating steps 5, and be incubated;
Step 7: product in filtration reactor, collects aluminum oxide filter cake, and dry.
2. the method for purification of aluminum oxide according to claim 1, is characterized in that, also comprises in described step 3 and described step 7: before to described aluminum oxide filtration cakes torrefaction, with scavenging solution repeated washing aluminum oxide filter cake 1-8 time.
3. the method for purification of aluminum oxide according to claim 1, is characterized in that, in described step 2 and described step 6: be heated to 25 DEG C-85 DEG C to described reactor, soaking time is 10min-6h.
4. the method for purification of aluminum oxide according to claim 1, is characterized in that, in described step 4: the temperature of calcining described aluminum oxide filter cake is 600 DEG C-2000 DEG C.
5. the method for purification of aluminum oxide according to claim 4, is characterized in that, in described step 4: the temperature of calcining described aluminum oxide filter cake is 1300 DEG C-1800 DEG C.
6. the method for purification of aluminum oxide according to claim 1, is characterized in that, in described step 1 and described step 5: the quality of described aluminum oxide and described scavenging solution is 1:1 ~ 1:20 than scope.
7. the method for purification of the aluminum oxide according to any one of claim 1-6, it is characterized in that, described scavenging solution comprises deionized water, at least one in salts solution that inorganic acid solution, organic acid soln, organic basic solution, positively charged ion are nonmetallic ion, aromatic hydrocarbon.
8. the method for purification of a kind of aluminum oxide according to claim 7, is characterized in that, also comprises at least one in oxygenant, reductive agent, complexing agent in described scavenging solution.
9. the method for purification of aluminum oxide according to claim 1, it is characterized in that, described reactor is any one in 316L stainless steel reactor, PE reactor, PP reactor, tetrafluoroethylene reactor, enamel reactor, 316L stainless steel lined PE reactor, 316L stainless steel lined PP reactor, 316L stainless steel lined tetrafluoroethylene reactor.
10. the method for purification of aluminum oxide according to claim 9, is characterized in that, described reactor is tetrafluoroethylene reactor.
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| CN110395757A (en) * | 2019-09-05 | 2019-11-01 | 东北大学 | A method of alkalies and alkaline earth impurity in removal acid oxidation aluminium |
| CN111170344A (en) * | 2020-01-15 | 2020-05-19 | 珠海琴晟新材料有限公司 | Preparation method of ultra-pure nano material |
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| CN102070169A (en) * | 2010-12-15 | 2011-05-25 | 中国铝业股份有限公司 | Preparation method of low-sodium active aluminum oxide |
| CN102910659A (en) * | 2012-10-29 | 2013-02-06 | 上海飞凯光电材料股份有限公司 | Preparation method and application of high-purity aluminum oxide |
| CN103204530A (en) * | 2013-05-14 | 2013-07-17 | 昆明冶金研究院 | Method for removing sodium in preparation of high-purity alumina |
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| CN101588993A (en) * | 2006-12-15 | 2009-11-25 | 日本轻金属株式会社 | Process for producing high-purity alpha-alumina |
| CN102070169A (en) * | 2010-12-15 | 2011-05-25 | 中国铝业股份有限公司 | Preparation method of low-sodium active aluminum oxide |
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| CN110395757B (en) * | 2019-09-05 | 2021-11-30 | 东北大学 | Method for removing alkali metal and alkaline earth metal impurities in acid-process alumina |
| CN111170344A (en) * | 2020-01-15 | 2020-05-19 | 珠海琴晟新材料有限公司 | Preparation method of ultra-pure nano material |
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