CN104030330B - 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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- CN104030330B CN104030330B CN201410265492.7A CN201410265492A CN104030330B CN 104030330 B CN104030330 B CN 104030330B CN 201410265492 A CN201410265492 A CN 201410265492A CN 104030330 B CN104030330 B CN 104030330B
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Abstract
The invention belongs to the field of high-purity aluminum hydroxide materials and provides a method for preparing high-purity aluminum hydroxide through induced crystallization. The method comprises the following steps: reacting high-purity aluminum with electronic-grade organic base and high-purity water to generate an aluminum-containing complex salt, adding a seed crystal to perform induced crystallization, decomposing the aluminum-containing complex salt into aluminum hydroxide and organic base; filtering the obtained aluminum hydroxide, washing and drying to prepare the high-purity aluminum hydroxide crystal with high purity and in a consistent crystal form, wherein the organic base is recycled. The method has the advantages of short process, use of readily available 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 percent, and the content of the impurities such as Fe, Si and Na is less than 3ppmw. The product high-purity aluminum hydroxide is particularly applied to the fields of high-purity aluminum oxide, light-emitting diode (LED) sapphire and luminous materials.
Description
Technical field
The invention belongs to chemical products preparation field is and in particular to a kind of prepare the consistent height of crystal formation by inducing crystallization technique
The preparation method of pure cerium hydroxide aluminum.More particularly it relates to it is a kind of using high-purity aluminum foil and electron level organic base and high-purity
Water reaction generates and contains aluminium double salts, induces crystallization by crystal seed, decomposes containing aluminium double salts and generates aluminum hydroxide crystals and organic base,
By the aluminium hydroxide obtaining through filtering, washing, the consistent high purity aluminium hydroxide crystal of crystal formation is prepared in drying, and organic base circulates
Using method.
Background technology
Crystallization is a kind of precipitation crystalline solid from liquid (solution or fused mass) or gaseous feed, belongs to heat, matter transmission
The unit operation of process.Crystallization process be macroscopically one from air-liquid or solid phase to the complicated phase transition process of solid phase, microcosmic is
A lot of atoms, ion, molecule or molecule group are aligned to the process in a regular three-dimensional periodic array by one, are one
The result of mass transfer between individual complicated multi phase state system.According to the feature of liquid-solid equilibrium, crystallization operation can not only take from solution
Obtain solid solute, and high-purity or ultrapure crystalline substance can be isolated from the mixture of the considerable solution of impurity or multicomponent
Body.The properties such as the form of crystal, size and purity not only play the role of important in crystal growth, but also decide product
The application of thing crystal.But crystal growth is a complicated process, is easily affected by several factors.Specific in order to obtain
Crystal, can be using anthropic factor controlling the growth course of crystal, i.e. induction crystallization.Induction crystallization is to be crystallized by analysis
Mechanism, controls the factor of impact crystallization process, forms specific physicochemical environment, and regulation and control nucleation and crystal growth two are important
Step, strengthening and the general designation controlling crystallization process method.Inducing crystallization technique is mainly used in material purifying with functionalization and to be become
One of main development direction.
High purity aluminium hydroxide has a wide range of applications.Aluminium hydroxide have fire-retardant, eliminate smoke, filling etc. function can serve as hinder
Combustion agent.High purity aluminium hydroxide can prepare high purity aluminium oxide, and then prepares sapphire etc..The purity of aluminum hydroxide crystals, crystal formation
The field of being applied to has decisive role.
The main technique preparing high purity aluminium hydroxide at present is alkoxide hydrolysis, including active aluminium alcoholates method and choline method etc..
(1) aluminium alcoholates method is SUMITOMO CHEMICAL patented technology, is carried out in two steps, first the Organic Alcohol such as aluminum and isopropanol reaction life
Become alcohol aluminium salt, alcohol aluminium salt removes through rectification becomes high-purity alcohol aluminium salt after excessive Organic Alcohol, and finally hydrolysis obtains aluminium hydroxide.Its
Shortcoming is: process route is long, and the reaction of alcohol and aluminum must be carried out in anhydrous conditions, under conditions of water exists, can significantly press down
Aluminum processed and the reaction of alcohol.In addition rectification is needed to reclaim Organic Alcohol, the operation such as membrane filtration impurity, equipment investment is big.
(2) choline method is aluminum and acetylcholine response generates double salt, and under supersaturated condition, the choline double salt hydrolysis of aluminum generates
Aluminium hydroxide simultaneously releases hydrogen.Chinese patent cn02108991.4 and Chinese patent 200510028367.5 all disclose this side
Method.But high-purity choline is needed to be refined by choline chloride ionic energy transfer and obtains, and choline purity is difficult to ensure card, therefore high-purity gallbladder
The acquisition of alkali determines product quality and cost.
Content of the invention
The purpose of the present invention be for existing high purity aluminium hydroxide production method technical process in the presence of above-mentioned deficiency,
A kind of method by inducing crystallization to prepare high purity aluminium hydroxide is provided, purity height, the consistent High Purity Hydrogen of crystal formation can be prepared
Aluminium oxide, and energy shortened process, reduces cost, environmental protection.
The new method that high purity aluminium hydroxide is prepared in a kind of induction crystallization proposed by the present invention is to add by the following technical programs
With realize:
A kind of method that high purity aluminium hydroxide is prepared in induction crystallization, using high-purity aluminum foil and electron level organic base and high purity water
Reaction generates and contains aluminium double salts, induces crystallization by crystal seed, decomposes containing aluminium double salts and generates aluminum hydroxide crystals and organic base, will
The aluminium hydroxide obtaining, through filtering, washs, and the consistent high purity aluminium hydroxide crystal of crystal formation, organic base circulation profit are prepared in drying
With comprising the steps:
(1) high-purity aluminum foil is added in the mixed solution of electron level organic base, high purity water, makes organic alkali concn after mixing
For 0.1mol/l～3mol/l, stirring reaction；
(2) high purity aluminium hydroxide crystal seed is added in (1) hybrid reaction system stage by stage；
(3) heterogeneous system having reacted (2) carries out solid-liquid separation, obtains pressed powder and mixed solution；
(4) with the pressed powder of high-purity water washing (3) gained, then process is dried to solid.
The method preparing high purity aluminium hydroxide by described induction crystallization, the wherein purity of high-purity aluminum foil be 99.999% with
On, aluminum foil thickness≤40 μm.
The method preparing high purity aluminium hydroxide by described induction crystallization, wherein electron level organic base are tetramethyl hydroxide
The mixture of one or more of ammonium, tetraethyl ammonium hydroxide, TPAOH.
By the described method inducing crystallization to prepare high purity aluminium hydroxide, the addition of wherein high purity aluminium hydroxide crystal seed is
The 10%～100% of product aluminium hydroxide weight.
The method preparing high purity aluminium hydroxide by described induction crystallization, wherein (2nd) step reaction system temperature is 50
～95 DEG C, the response time is 1～8 hour.
The method preparing high purity aluminium hydroxide by described induction crystallization, the wherein organic alkali concn of electron level are 0.1mol/l
～3mol/l, and recycle.
The method preparing high purity aluminium hydroxide by described induction crystallization, wherein aluminium hydroxide are filtered into centrifugation or true
Empty filtration.
The method preparing high purity aluminium hydroxide by described induction crystallization, wherein aluminium hydroxide baking temperature are 100～250
℃.
The method preparing high purity aluminium hydroxide by described induction crystallization, wherein high-purity water resistivity are >=15m ω
cm..
The present invention is directed to the deficiencies in the prior art, by reacting life using high-purity aluminum foil with electron level organic base and high purity water
Become to contain aluminium double salts, crystallization is induced by crystal seed, decompose containing aluminium double salts and generate aluminum hydroxide crystals and organic base, by obtain
Aluminium hydroxide, through filtering, washs, and the consistent high purity aluminium hydroxide crystal of crystal formation is prepared in drying.
The ultimate principle of the new method of the present invention is as follows:
Hydrolysis: al+roh+3h2o→r[al(oh)4]+1.5h2
Induction crystallization:
The process characteristic of the new method of the present invention is as follows:
1st, flow process is short: compares aluminium alcoholates method, this technique is used, greatly shortened by rafifinal and water direct reaction, Recycling Mother Solution
Technological process, and mother solution is not required to rectification and purification.
2nd, raw material is easy to get: compared with choline method, high-purity specially good effect organic base that this project adopts easily obtains, can be commercially
Convenient purchase, and purity is high, and all metal ions are less than 10ppb it is ensured that product quality.
3rd, low cost: this technique achieves aluminum and water direct reaction and generates high purity aluminium hydroxide, equipment operation mild condition,
Because catalyst recycles, consumption is little, so overall cost is less than aluminium alcoholates method and choline method.
4th, pollution-free: in technique, primary raw material is water and aluminum, product is aluminium hydroxide and hydrogen, and a large amount of hydrogen of generation can
To recycle.There is no any waste residue, waste water, waste gas discharge.
Compared with prior art, the induction crystallization that the present invention provides is prepared high purity aluminium hydroxide technique and is had excellent benefit as follows
Property:
(1) crystallized by induction, product purity height (99.999%), the constituent content such as fe, si, na is respectively less than 3ppm.And
And, crystal formation is α aluminium hydroxide.
(2) low cost, generation technical process requirement is low, and operating condition is gentle.
(3) organic base can recycle, and consumption is little, low production cost.
(4) flow process is short: compares aluminium alcoholates method, this technique is used by aluminum and water direct reaction, Recycling Mother Solution, substantially reduces work
Skill flow process, and mother solution is not required to rectification and purification.
(5) pollution-free: in technique, primary raw material is water and aluminum, product is aluminium hydroxide and hydrogen, a large amount of hydrogen of generation
Can recycle.There is no any waste residue, waste water, waste gas discharge.
Brief description
Fig. 1 is the process chart 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 induction crystallized product；
Fig. 5 is the xrd material phase analysis of induction crystallized product.
Specific embodiment
Below in conjunction with the accompanying drawings, outstanding advantages and the innovative point of the present invention is further illustrated by the embodiment of the present invention, but
The present invention is not limited with this.
Embodiment 1
In politef reactor, concentration is 3mol/l to the organic base taking 300ml, and arranges agitator speed and be
240rpm, reaction temperature is 70 DEG C, adds 5g aluminium foil to be hydrolyzed reaction, is simultaneously introduced gibbsite crystal seed and carries out induction and ties
Crystalline substance, seed load is 1.45g, 1 hour reactive crystallization time.The al (oh) that will be generated with high speed centrifuge3With reaction reagent
Separate, and be neutral with high-purity water washing pressed powder to washing liquid, put in the drying baker that temperature is 100 DEG C and be dried.Produce
Product aluminium hydroxide quality is 14.4g, and crystal formation is α-al (oh)3, its impurity content the results are shown in Table 1.
Table 1 induces crystallized product purity analysis
| Impurity | fe | si | na | mg | ni | ti | zn | cu | c |
| ppm | 2 | 2 | 1 | 0.2 | 0.1 | 0.1 | 0.2 | ----- | ----- |
Embodiment 2
Take 10ml organic base (3mol/l) and 290ml high purity water in politef reactor, speed of agitator is
240rpm, reaction temperature is 95 DEG C, adds 5g aluminium foil to be hydrolyzed reaction, is simultaneously introduced gibbsite crystal seed and carries out induction and ties
Crystalline substance, seed load is 14.4g, 8 hours reactive crystallization time.After reaction terminates, carry out sucking filtration with vacuum pump, and use high purity water
Washing crystal is neutrality to washing liquid, is dried in the drying baker being subsequently placed in 250 DEG C.Product aluminium hydroxide quality is 15.0g,
Crystal formation is α-al (oh)3, its impurity content the results are shown in Table 2.
Table 2 induces crystallized product purity analysis
| 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
Take 100ml organic base (3mol/l) and 200ml high purity water in politef reactor, speed of agitator is
240rpm, reaction temperature is 90 DEG C, adds 5g aluminium foil to be hydrolyzed reaction, is simultaneously introduced gibbsite crystal seed and carries out induction and ties
Crystalline substance, seed load is 14.4g, 4 hours reactive crystallization time.After reaction terminates, carry out sucking filtration with vacuum pump, and use high purity water
Washing crystal is neutrality to washing liquid, is dried in the drying baker being subsequently placed in 250 DEG C.Product aluminium hydroxide quality is 14.5g,
Crystal formation is α-al (oh)3, its impurity content the results are shown in Table 3.
Table 3 induces crystallized product purity analysis
| 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
Take 50ml organic base (3mol/l) and 200ml high purity water in politef reactor, speed of agitator is
240rpm, reaction temperature is 80 DEG C, adds 5g aluminium foil to be hydrolyzed reaction, is simultaneously introduced gibbsite crystal seed and carries out induction and ties
Crystalline substance, seed load is 7.222g, 3 hours reactive crystallization time.After reaction terminates, carry out sucking filtration with vacuum pump, and with high-purity
Water washing crystal is neutrality to washing liquid, is dried in the drying baker being subsequently placed in 250 DEG C.Product aluminium hydroxide quality is
14.8g, crystal formation is α-al (oh)3, its impurity content the results are shown in Table 4.
Table 4 induces crystallized product purity analysis
| 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
Take 50ml organic base (3mol/l) and 200ml high purity water in politef reactor, speed of agitator is
240rpm, reaction temperature is 50 DEG C, adds 5g aluminium foil to be hydrolyzed reaction, is simultaneously introduced gibbsite crystal seed and carries out induction and ties
Crystalline substance, seed load is 7.2g, 5 hours reactive crystallization time.After reaction terminates, carry out sucking filtration with vacuum pump, and use high purity water
Washing crystal is neutrality to washing liquid, is dried in the drying baker being subsequently placed in 250 DEG C.Product aluminium hydroxide quality is 14.8g,
Crystal formation is α-al (oh)3, its impurity content the results are shown in Table 5.
Table 5 induces crystallized product purity analysis
| 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 (2)
1. a kind of induction crystallization prepare high purity aluminium hydroxide method it is characterised in that:
Generation is reacted using high-purity aluminum foil and electron level organic base and high purity water and contains aluminium double salts, crystallization is induced by crystal seed,
Decompose containing aluminium double salts and generate aluminum hydroxide crystals and organic base, by the aluminium hydroxide obtaining through filtering, washing, drying is prepared
The consistent high purity aluminium hydroxide crystal of crystal formation, organic base recycles, and comprises the steps:
(1) high-purity aluminum foil is added in the mixed solution of electron level organic base, high purity water, after making mixing, organic alkali concn is
0.1mol/l～3mol/l, stirring reaction；The purity of described high-purity aluminum foil is more than 99.999%, aluminum foil thickness≤40 μm；Institute
Stating electron level organic base is one or more of Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH
Mixture, the organic alkali concn of described electron level is 0.1mol/l～3mol/l, and recycles；
(2) high purity aluminium hydroxide crystal seed is added in (1) hybrid reaction system stage by stage, described high purity aluminium hydroxide crystal seed
Addition is the 10%～100% of new crystalline product aluminium hydroxide weight, and temperature of reaction system is 50～95 DEG C, and the response time is 1
～8 hours；
(3) heterogeneous system having reacted (2) carries out solid-liquid separation, with centrifugation or vacuum filter, obtain pressed powder and
Mixed solution；
(4) with the pressed powder of high-purity water washing (3) gained, then solid is dried with process, baking temperature be 100～
250℃；
Described high-purity water resistivity is >=15m ω cm.
2. a kind of induction crystallization prepares the method for high purity aluminium hydroxide it is characterised in that taking 300ml's as claimed in claim 1
In politef reactor, concentration is 3mol/l to organic base, and arranges agitator speed for 240rpm, and reaction temperature is
70 DEG C, add 5g aluminium foil to be hydrolyzed reaction, be simultaneously introduced high purity aluminium hydroxide crystal seed and carry out induction and crystallize, seed load is
1.45g, 1 hour reactive crystallization time, the al (oh) that will be generated with high speed centrifuge3Separate with reaction reagent, and use high purity water
Washing pressed powder is neutrality to washing liquid, puts in the drying baker that temperature is 100 DEG C and is dried, product aluminium hydroxide quality is
14.4g, crystal formation is α-al (oh)3, its impurity content the results are shown in Table 1:
Table 1 induces crystallized product purity analysis
.
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| RU2114785C1 (en) * | 1997-05-15 | 1998-07-10 | Общество с ограниченной ответственностью "ИВТЕХИМ" | Method for production of aluminium hydroxide |
| CN1903728A (en) * | 2005-07-29 | 2007-01-31 | 中国科学院上海硅酸盐研究所 | Preparation method of high purity aluminium oxide powder |
| CN101575110A (en) * | 2008-05-09 | 2009-11-11 | 大连路明纳米材料有限公司 | Preparation method of alumina powder |
| CN103523810A (en) * | 2012-07-04 | 2014-01-22 | 何礼君 | Preparation method of high-purity aluminum oxide |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1074751C (en) * | 1997-11-21 | 2001-11-14 | 淄博兆亿保健用品实业有限公司 | Production method of rare earth nitrate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2114785C1 (en) * | 1997-05-15 | 1998-07-10 | Общество с ограниченной ответственностью "ИВТЕХИМ" | Method for production of aluminium hydroxide |
| CN1903728A (en) * | 2005-07-29 | 2007-01-31 | 中国科学院上海硅酸盐研究所 | Preparation method of high purity aluminium oxide powder |
| CN101575110A (en) * | 2008-05-09 | 2009-11-11 | 大连路明纳米材料有限公司 | Preparation method of alumina powder |
| CN103523810A (en) * | 2012-07-04 | 2014-01-22 | 何礼君 | Preparation method of high-purity aluminum oxide |
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