CN104030330A - Method for preparing high-purity aluminum hydroxide through induced crystallization - Google Patents
Method for preparing high-purity aluminum hydroxide through induced crystallization Download PDFInfo
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- CN104030330A CN104030330A CN201410265492.7A CN201410265492A CN104030330A CN 104030330 A CN104030330 A CN 104030330A CN 201410265492 A CN201410265492 A CN 201410265492A CN 104030330 A CN104030330 A CN 104030330A
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- aluminium hydroxide
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- induced crystallization
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 68
- 238000002425 crystallisation Methods 0.000 title claims abstract description 58
- 230000008025 crystallization Effects 0.000 title claims abstract description 56
- 239000013078 crystal Substances 0.000 claims abstract description 55
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 38
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 150000007530 organic bases Chemical class 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 21
- 239000012498 ultrapure water Substances 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 17
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 5
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 60
- 239000004411 aluminium Substances 0.000 claims description 25
- 230000015572 biosynthetic process Effects 0.000 claims description 17
- 239000011888 foil Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 2
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000001939 inductive effect Effects 0.000 abstract description 3
- 229910052594 sapphire Inorganic materials 0.000 abstract description 2
- 239000010980 sapphire Substances 0.000 abstract description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- 229960001231 choline Drugs 0.000 description 8
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000005030 aluminium foil Substances 0.000 description 5
- 229910001679 gibbsite Inorganic materials 0.000 description 5
- 239000006210 lotion Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 5
- 229910018626 Al(OH) Inorganic materials 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 101100352919 Caenorhabditis elegans ppm-2 gene Proteins 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 1
- 235000019743 Choline chloride Nutrition 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- OIPILFWXSMYKGL-UHFFFAOYSA-N acetylcholine Chemical compound CC(=O)OCC[N+](C)(C)C OIPILFWXSMYKGL-UHFFFAOYSA-N 0.000 description 1
- 229960004373 acetylcholine Drugs 0.000 description 1
- 150000004703 alkoxides Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229960003178 choline chloride Drugs 0.000 description 1
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明属于高纯氧化铝材料领域，提供一种诱导结晶制备高纯氢氧化铝的方法。该方法采用高纯铝与电子级有机碱、高纯水反应生成的含铝复盐，通过添加晶种诱导结晶，含铝复盐分解得到氢氧化铝和有机碱，将得到的氢氧化铝经过过滤，洗涤，干燥制备出纯度高、晶型一致的高纯氢氧化铝晶体，有机碱可循环利用。该方法流程短、原料易得、产品质量高、成本低、无污染。所得氢氧化铝粉体的纯度为≥99.999％，Fe、Si、Na等杂质含量均小于3ppmw。产品高纯氢氧化铝特别适用于高纯氧化铝，LED蓝宝石、发光材料等领域。
The invention belongs to the field of high-purity alumina materials and provides a method for inducing crystallization to prepare high-purity aluminum hydroxide. The method adopts the aluminum-containing double salt generated by the reaction of high-purity aluminum, electronic-grade organic base and high-purity water. By adding seeds to induce crystallization, the aluminum-containing double salt is decomposed to obtain aluminum hydroxide and organic base, and the obtained aluminum hydroxide is filtered. Washing and drying produce high-purity aluminum hydroxide crystals with high purity and consistent crystal form, and the organic base can be recycled. The method has the advantages of short process flow, easy-to-obtain raw materials, high product quality, low cost and no pollution. The purity of the obtained aluminum hydroxide powder is more than or equal to 99.999%, and the contents of impurities such as Fe, Si and Na are all less than 3ppmw. The product high-purity aluminum hydroxide is especially suitable for high-purity alumina, LED sapphire, luminescent materials and other fields.
Description
Technical field
The invention belongs to Chemicals preparation field, be specifically related to a kind of preparation method who prepares the consistent high purity aluminium hydroxide of crystal formation by inducing crystallization technique.More specifically, the present invention relates to a kind of employing high-purity aluminum foil and react generation with electronic-grade organic bases and high purity water containing aluminium double salts, by the effect of crystal seed induced crystallization, containing aluminium double salts, decompose and generate aluminum hydroxide crystals and organic bases, the aluminium hydroxide process obtaining is filtered, washing, the dry consistent high purity aluminium hydroxide crystal of crystal formation, the method for organic bases recycle prepared.
Background technology
Crystallization be a kind of from liquid (solution or melts) or gaseous feed crystallize out material, belong to the unit operation of heat, matter transmittance process.It in crystallisation process macroscopic view, is a complicated phase transition process from gas, liquid or solid phase to solid phase, on microcosmic, being one a lot of atoms, ion, molecule or molecule group are aligned to a process in regular three-dimensional periodic array, is the result of mass transfer between a complicated multi phase state system.According to the feature of liquid-solid equilibrium, crystallization operation not only can be obtained solid solute from solution, and can from the mixture of the considerable solution of impurity or multicomponent, isolate high-purity or ultrapure crystal.The form of crystal, the character such as size and purity not only have important effect in crystal auxology, but also are determining the application of product crystal.But crystal growth is a complicated process, is easily subject to the impact of several factors.In order to obtain specific crystal, can adopt human factor to control the process of growth of crystal, i.e. induced crystallization.Induced crystallization is that the factor of control effect crystallisation process, forms specific physicochemical environment by analyzing crystallization mechanism, regulation and control nucleation and two important steps of crystal growth, the general designation of strengthening and crystallization control process approach.Inducing crystallization technique is mainly used in material purifying and functionalization and becomes one of main development direction.
High purity aluminium hydroxide has a wide range of applications.The functions such as that aluminium hydroxide has is fire-retardant, smoke elimination, filling can be used as fire retardant.High purity aluminium hydroxide can be prepared high purity aluminium oxide, and then prepares sapphire etc.The purity of aluminum hydroxide crystals, crystal formation have decisive role to its Application Areas.
The main technique of preparing at present high purity aluminium hydroxide is alkoxide hydrolysis, comprises active aluminium alcoholates method and choline method etc.
(1) aluminium alcoholates method is SUMITOMO CHEMICAL patented technology, carries out in two steps, and first the reaction of the Organic Alcohol such as aluminium and Virahol generates aluminium alcoholates salt, and aluminium alcoholates salt becomes high-purity aluminium alcoholates salt after excessive Organic Alcohol is removed in rectifying, and finally hydrolysis obtains aluminium hydroxide.Its shortcoming is: operational path is long, and the reaction of alcohol and aluminium must be carried out under anhydrous condition, under the condition existing, can greatly suppress the reaction of aluminium and alcohol at water.In addition need rectifying to reclaim Organic Alcohol, the operations such as membrane filtration impurity, facility investment is large.
(2) choline method is that aluminium and acetylcholine response generate double salt, and under supersaturated condition, the hydrolysis of the choline double salt of aluminium generates aluminium hydroxide releasing hydrogen gas.Chinese patent CN02108991.4 and Chinese patent 200510028367.5 all disclose this method.But high-purity choline need to obtain by choline chloride 60 ion-exchange separation and purification, and choline purity is difficult to ensure card, therefore the acquisition of high-purity choline has determined quality product and cost.
Summary of the invention
The object of the invention is for existing above-mentioned deficiency in existing high purity aluminium hydroxide production method technological process, a kind of method of preparing high purity aluminium hydroxide by induced crystallization is provided, purity can be prepared high, the high purity aluminium hydroxide that crystal formation is consistent, again can shortened process, reduce costs environmental protection.
The novel method that a kind of induced crystallization that the present invention proposes is prepared high purity aluminium hydroxide is realized by the following technical programs:
A kind of induced crystallization is prepared the method for high purity aluminium hydroxide, adopt high-purity aluminum foil to react with electronic-grade organic bases and high purity water and generate containing aluminium double salts, by the effect of crystal seed induced crystallization, containing aluminium double salts, decompose and generate aluminum hydroxide crystals and organic bases, by the aluminium hydroxide obtaining, through filtering, washing, is dried and prepares the consistent high purity aluminium hydroxide crystal of crystal formation, organic bases recycle, comprises the steps:
(1) high-purity aluminum foil is joined in the mixing solutions of electronic-grade organic bases, high purity water, making to mix rear organic bases concentration is 0.1mol/L～3mol/L, stirring reaction;
(2) high purity aluminium hydroxide crystal seed is joined stage by stage in (1) hybrid reaction system;
(3) heterogeneous system (2) having been reacted carries out solid-liquid separation, obtains pressed powder and mixing solutions;
(4) with the pressed powder of high purity water washing (3) gained, then solid is carried out to drying treatment.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein the purity of high-purity aluminum foil is more than 99.999%, aluminum foil thickness≤40 μ m.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein electronic-grade organic bases is one or more the mixture in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein the addition of high purity aluminium hydroxide crystal seed is 10%～100% of product aluminium hydroxide weight.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein (2) step reaction system temperature is 50～95 ℃, the reaction times is 1～8 hour.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein electronic-grade organic bases concentration is 0.1mol/L～3mol/L, and recycle.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein aluminium hydroxide is filtered into centrifugation or vacuum filtration.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein aluminium hydroxide drying temperature is 100～250 ℃.
The method of preparing high purity aluminium hydroxide by described induced crystallization, wherein high-purity water resistivity is >=15M Ω cm..
The present invention is directed to the deficiencies in the prior art, by adopting high-purity aluminum foil to react with electronic-grade organic bases and high purity water, generate containing aluminium double salts, by the effect of crystal seed induced crystallization, containing aluminium double salts, decompose and generate aluminum hydroxide crystals and organic bases, the aluminium hydroxide process obtaining is filtered, washing, the dry consistent high purity aluminium hydroxide crystal of crystal formation of preparing.
The ultimate principle of novel method of the present invention is as follows:
Hydrolysis reaction: Al+ROH+3H
2o → R[Al (OH)
4]+1.5H
2
Induced crystallization:
The process characteristic of novel method of the present invention is as follows:
1, flow process is short: compare aluminium alcoholates method, this technique is by rafifinal and water direct reaction, and Recycling Mother Solution is used, and greatly shortened technical process, and mother liquor does not need rectification and purification.
2, raw material is easy to get: compare with choline method, high-purity special efficacy organic bases that this project adopts easily obtains, and can on market, conveniently purchase, and purity is high, and all metal ions is less than 10ppb, has guaranteed quality product.
3, cost is low: this technique has realized aluminium and water direct reaction and generated high purity aluminium hydroxide, operation of equipment mild condition, because catalyst recirculation is used, consumption seldom, so overall cost is lower than aluminium alcoholates method and choline method.
4, pollution-free: in technique, main raw material is water and aluminium, product is aluminium hydroxide and hydrogen, and a large amount of hydrogen of generation can be recycled.Without any waste residue, waste water, exhaust gas emission.
Compared with prior art, induced crystallization provided by the invention is prepared high purity aluminium hydroxide technique and is had following excellent benefit:
(1) by induced crystallization, product purity high (99.999%), the constituent contents such as Fe, Si, Na are all less than 3ppm.And crystal formation is α aluminium hydroxide.
(2) cost is low, and it is low that generating process is crossed range request, and operational condition is gentle.
(3) organic bases can recycle, and seldom, production cost is low for consumption.
(4) flow process is short: compare aluminium alcoholates method, this technique is by aluminium and water direct reaction, and Recycling Mother Solution is used, and greatly shortened technical process, and mother liquor does not need rectification and purification.
(5) pollution-free: in technique, main raw material is water and aluminium, product is aluminium hydroxide and hydrogen, and a large amount of hydrogen of generation can be recycled.Without any waste residue, waste water, exhaust gas emission.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the SEM photo of aluminium hydroxide crystal seed;
Fig. 3 is the XRD material phase analysis of aluminium hydroxide crystal seed;
Fig. 4 is the SEM photo of induced crystallization product;
Fig. 5 is the XRD material phase analysis of induced crystallization product.
Embodiment
Below in conjunction with accompanying drawing, by the furthermore bright outstanding advantages of the present invention of the embodiment of the present invention and innovative point, but with this, do not limit the present invention.
Embodiment 1
Get the organic bases of 300mL in tetrafluoroethylene reactor, concentration is 3mol/L, and it is 240rpm that agitator speed is set, temperature of reaction is 70 ℃, add the reaction that is hydrolyzed of 5g aluminium foil, add gibbsite crystal seed to carry out induced crystallization, seed load is 1.45g simultaneously, 1 hour reactive crystallization time.With supercentrifuge by the Al (OH) generating
3separated with reaction reagent, and be neutral by high purity water washing pressed powder to washing lotion, the loft drier of putting into temperature and be 100 ℃ is dried.Product aluminium hydroxide quality is 14.4g, and crystal formation is α-Al (OH)
3, its foreign matter content the results are shown in Table 1.
Table 1 induced crystallization product purity is analyzed
| Impurity | Fe | Si | Na | Mg | Ni | Ti | Zn | Cu | C |
| ppm | 2 | 2 | 1 | 0.2 | 0.1 | 0.1 | 0.2 | ----- | ----- |
Embodiment 2
Get 10mL organic bases (3mol/L) and 290mL high purity water in tetrafluoroethylene reactor, mixing speed is 240rpm, temperature of reaction is 95 ℃, add the reaction that is hydrolyzed of 5g aluminium foil, add gibbsite crystal seed to carry out induced crystallization simultaneously, seed load is 14.4g, 8 hours reactive crystallization time.After reaction finishes, with vacuum pump, carry out suction filtration, and be neutrality by high purity water washing crystal to washing lotion, be then placed in the loft drier of 250 ℃ and be dried.Product aluminium hydroxide quality is 15.0g, and crystal formation is α-Al (OH)
3, its foreign matter content the results are shown in Table 2.
Table 2 induced crystallization product purity is analyzed
| Crystal formation | Impurity | Fe | Si | Na | Mg | Ni | Ti | Zn | Cu | C | Other Other |
| α-Al(OH) 3 | ppm | 1 | 1 | 0.5 | 0.1 | 0.1 | 0.1 | 0.1 | ----- | ----- | 1 |
Embodiment 3
Get 100mL organic bases (3mol/L) and 200mL high purity water in tetrafluoroethylene reactor, mixing speed is 240rpm, temperature of reaction is 90 ℃, add the reaction that is hydrolyzed of 5g aluminium foil, add gibbsite crystal seed to carry out induced crystallization simultaneously, seed load is 14.4g, 4 hours reactive crystallization time.After reaction finishes, with vacuum pump, carry out suction filtration, and be neutrality by high purity water washing crystal to washing lotion, be then placed in the loft drier of 250 ℃ and be dried.Product aluminium hydroxide quality is 14.5g, and crystal formation is α-Al (OH)
3, its foreign matter content the results are shown in Table 3.
Table 3 induced crystallization product purity is analyzed
| Crystal formation | Impurity | Fe | Si | Na | Mg | Ni | Ti | Zn | Cu | C | Other Other |
| α-Al(OH) 3 | ppm | 2 | 2 | 1 | 0.5 | 0.1 | 0.1 | 0.2 | ----- | ----- | 1 |
Embodiment 4
Get 50mL organic bases (3mol/L) and 200mL high purity water in tetrafluoroethylene reactor, mixing speed is 240rpm, temperature of reaction is 80 ℃, add the reaction that is hydrolyzed of 5g aluminium foil, add gibbsite crystal seed to carry out induced crystallization simultaneously, seed load is 7.222g, 3 hours reactive crystallization time.After reaction finishes, with vacuum pump, carry out suction filtration, and be neutrality by high purity water washing crystal to washing lotion, be then placed in the loft drier of 250 ℃ and be dried.Product aluminium hydroxide quality is 14.8g, and crystal formation is α-Al (OH)
3, its foreign matter content the results are shown in Table 4.
Table 4 induced crystallization product purity is analyzed
| Crystal formation | Impurity | Fe | Si | Na | Mg | Ni | Ti | Zn | Cu | C | Other Other |
| α-Al(OH) 3 | ppm | 1.5 | 2 | 1 | 0.5 | 0.1 | 0.1 | 0.2 | ----- | ----- | 1 |
Embodiment 5
Get 50mL organic bases (3mol/L) and 200mL high purity water in tetrafluoroethylene reactor, mixing speed is 240rpm, temperature of reaction is 50 ℃, add the reaction that is hydrolyzed of 5g aluminium foil, add gibbsite crystal seed to carry out induced crystallization simultaneously, seed load is 7.2g, 5 hours reactive crystallization time.After reaction finishes, with vacuum pump, carry out suction filtration, and be neutrality by high purity water washing crystal to washing lotion, be then placed in the loft drier of 250 ℃ and be dried.Product aluminium hydroxide quality is 14.8g, and crystal formation is α-Al (OH)
3, its foreign matter content the results are shown in Table 5.
Table 5 induced crystallization product purity is analyzed
| Crystal formation | Impurity | Fe | Si | Na | Mg | Ni | Ti | Zn | Cu | C | Other Other |
| α-Al(OH) 3 | ppm | 1 | 2 | 1 | 0.5 | 0.1 | 0.1 | 0.2 | ----- | ----- | 1 |
Claims (9)
1. induced crystallization is prepared a method for high purity aluminium hydroxide, it is characterized in that:
Adopt high-purity aluminum foil to react with electronic-grade organic bases and high purity water and generate containing aluminium double salts, by the effect of crystal seed induced crystallization, containing aluminium double salts, decompose and generate aluminum hydroxide crystals and organic bases, the aluminium hydroxide process obtaining is filtered, washing, be dried and prepare the consistent high purity aluminium hydroxide crystal of crystal formation, organic bases recycle, comprises the steps:
(1) high-purity aluminum foil is joined in the mixing solutions of electronic-grade organic bases, high purity water, making to mix rear organic bases concentration is 0.1mol/L～3mol/L, stirring reaction;
(2) high purity aluminium hydroxide crystal seed is joined stage by stage in (1) hybrid reaction system;
(3) heterogeneous system (2) having been reacted carries out solid-liquid separation, obtains pressed powder and mixing solutions;
(4) with the pressed powder of high purity water washing (3) gained, then solid is carried out to drying treatment.
2. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, it is characterized in that the purity of described high-purity aluminum foil is more than 99.999%, aluminum foil thickness≤40 μ m.
3. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, it is characterized in that described electronic-grade organic bases is one or more the mixture in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH.
4. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, the addition that it is characterized in that described high purity aluminium hydroxide crystal seed is 10%～100% of product aluminium hydroxide weight.
5. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, it is characterized in that described (2) step reaction system temperature is 50～95 ℃, the reaction times is 1～8 hour.
6. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, it is characterized in that described electronic-grade organic bases concentration is 0.1mol/L～3mol/L, and recycle.
7. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, it is characterized in that described aluminium hydroxide is filtered into centrifugation or vacuum filtration.
8. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, it is characterized in that described aluminium hydroxide drying temperature is 100～250 ℃.
9. by induced crystallization claimed in claim 1, prepare the method for high purity aluminium hydroxide, it is characterized in that described high-purity water resistivity is >=15M Ω cm..
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113233487A (en) * | 2021-06-30 | 2021-08-10 | 包头交大赛福尔新材料有限公司 | Aluminum hydroxide and preparation method thereof |
| CN115974117A (en) * | 2022-12-20 | 2023-04-18 | 赵伟轩 | Preparation method and device of high-purity aluminum hydroxide and preparation method of high-purity aluminum oxide |
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| CN113233487A (en) * | 2021-06-30 | 2021-08-10 | 包头交大赛福尔新材料有限公司 | Aluminum hydroxide and preparation method thereof |
| CN113233487B (en) * | 2021-06-30 | 2022-09-20 | 上海交通大学包头材料研究院 | Aluminum hydroxide and preparation method thereof |
| CN115974117A (en) * | 2022-12-20 | 2023-04-18 | 赵伟轩 | Preparation method and device of high-purity aluminum hydroxide and preparation method of high-purity aluminum oxide |
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