CN1011882B - Prodn. sandy aluminium hydroxide - Google Patents
Prodn. sandy aluminium hydroxideInfo
- Publication number
- CN1011882B CN1011882B CN85105213A CN85105213A CN1011882B CN 1011882 B CN1011882 B CN 1011882B CN 85105213 A CN85105213 A CN 85105213A CN 85105213 A CN85105213 A CN 85105213A CN 1011882 B CN1011882 B CN 1011882B
- Authority
- CN
- China
- Prior art keywords
- decomposition
- seed
- aluminium hydroxide
- sandy
- branch
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/185—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process of crystalline silica-polymorphs having molecular sieve properties, e.g. silicalites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/16—After treatment, characterised by the effect to be obtained to increase the Si/Al ratio; Dealumination
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to an emthdo for preparing aluminium hydroxide from sodium aluminate solution, which mainly solves two problems that the decomposition rate of seed decomposition for preparing sandy aluminium hydroxide in a combined method or a sintering method is low, and carbonization decomposition can not prepare the sandy aluminium hydroxide. The present invention adopts prior seed decomposition, seed carbonization decomposition and post seed decomposition, namely that the powdery aluminium hydroxide prepared in the prior seed decomposition is used as seed crystals of seed carbonization decomposition, the products of the seed carbonization decomposition is used as seed crystals for the post seed decomposition, and finally the sandy aluminium hydroxide of the prior seed decomposition and post seed decomposition is sintered into a single sandy alumina. The decomposition rate of two kinds of the seed decomposition can reach 50%. The present invention can be used for factories for preparing sandy alumina from empholite monohydrate ore.
Description
The invention belongs to the method for from sodium aluminate solution, producing sandy aluminium hydroxide.
Industrial production method of alumina mainly contains bayer's process and sintering process, and these two kinds of methods respectively have its advantage and the scope of application.Under certain conditions, adopt the combination producing flow process of bayer's process and sintering process, can take in the advantage of two kinds of methods concurrently, obtain the better economical effectiveness of more single bayer's process or sintering process, simultaneously resource is utilized more fully.The ultimate principle of the whole bag of tricks is seen " process for making alumina " (Yang Chongyu of Central-South China Institute of Mining and Metallurgy chief editor), and can there be some variations in each factory according to s own situation Production Flow Chart and condition.
Since the seventies, sandy alumina production has become countries in the world aluminum oxide industry main development tendency.But bayer's process is all adopted in various countries' sandy alumina production at present, not useful as yet integrated process or sintering process.
Aluminum oxide grain size is mainly by the hydroxide particle-size decision, and hydroxide particle-size depends primarily on the method that aluminium hydroxide crystallizes out from oversaturated sodium aluminate solution, be commonly referred to as decomposition method and decomposition process and condition.The aluminium hydroxide that meets the sandy alumina requirement also should be the sand shape, and its granularity should be-44 μ＜7%, and after roasting gained aluminum oxide grain size-44 μ＜12%, specific surface area＞35m
2/ g, α-Al
2O
3Content is 20～30%.
Decomposition of crystal seed is to produce the passing method of sandy alumina.Produce sandy alumina technology comparative maturity in this way, it has many advantages to handling boehmite or gibbsite type aluminium ore.But with regard to prior art, plant to divide produce sandy alumina and exist kind of the not high shortcoming of branch rate of decomposition, the generalized case rate of decomposition is no more than 40%, that is to say that present kind is divided to produce sandy alumina and obtain as cost to sacrifice rate of decomposition.(seeing " light metal " 1981.4 phase P6 " sandy alumina ") is if will further improve rate of decomposition, for example bring up near 50%, the serious refinement of the aluminium hydroxide that then decomposites, after the classification, except that some is that sandy aluminium hydroxide product and a part of thin aluminium hydroxide return and is used as the seed, also have some granularity to account for 25～50% aluminium hydroxide for-44 μ, can only produce powdery aluminum uses, powdery aluminum can be used as industrial chemicals, powdery aluminum also is the raw material of electrolytic aluminum, but flies upward shortcomings such as loss is big.Therefore, the kind of prior art can not obtain single sandy aluminium hydroxide after dividing the raising rate of decomposition, and the kind of prior art divides the crystal seed that uses all to adopt kind of the aluminium hydroxide that branch self is produced (seeing " light metal " 1983.4P12).
The yellow soda ash batching that the sintering process employing is cheap feeds carbonic acid gas so adopt in a part of sodium aluminate in sintering process is produced, i.e. the method for carbonating decomposition is produced aluminium hydroxide, and carbon mother liquid can return the preparation charge pulp.The carbon branch of prior art also is not used in the production sandy aluminium hydroxide, and the carbon branch has carbon branch that does not add crystal seed and the carbon that adds crystal seed to divide other.Can improve the granularity of aluminium hydroxide with the carbon branch way that adds crystal seed.Soviet Union's magazine " non-ferrous metal " second phase in 1971 " aluminate solution adds the research that the carbon of crystal seed divides ", articles and opinions were stated: do not add the aluminate solution carbon branch of crystal seed, at the initial stage, aluminium hydroxide is separated out very slow, and the crystallization velocity of aluminium hydroxide is very fast when adding crystal seed.Utilizing the crystalline method can improve hydroxide particle-size forms.Experiment discloses, owing to utilize crystal seed, aluminium hydroxide crystal seed is grown up.Data shows, mainly is the rank of increase-100+60 μ, and reduces-40 μ grades.
The university teaching material that the Soviet Union published in 1978, introduce in " alumina producing " (second edition) that people such as Lan Er AulauHep compile, carbon branch temperature in Soviet Union factory is 70～80 ℃, and often add aluminium hydroxide crystal seed, carbon divides 6～8 hours time, carbon divides the aluminium hydroxide of gained thicker, and alkali content is low.The sintering process seminal fluid all enters the carbon branch in the Soviet Union factory, does not use kind of a branch, and adding kind of the crystal seed of carbon branch is that carbon branch self product is later made crystal seed, and seed is thicker, and the seed of use is than higher.Not add the aluminium hydroxide that crystal seed carbon divide to obtain thicker although add kind of carbon proportion by subtraction, prior art, and this aluminium hydroxide product does not also claim sandy aluminium hydroxide, does not reach the requirement of production sandy alumina.
Up to now, yet there are no and utilize kind of branch to produce-44 μ to account for the report that 25～50% fine-grained aluminum hydroxide is made carbonation decompsition seed crystal, also do not see to have and utilize the carbon branch to produce aluminium hydroxide to make kind of the report of the seed production sandy aluminium hydroxide that divides.
Produce the situation that the sandy aluminium hydroxide rate of decomposition is not high and integrated process can't be produced sandy aluminium hydroxide at kind of branch.Purpose of the present invention just is to provide a kind of integrated process factory that can be used for to decompose the method for producing sandy aluminium hydroxide from oversaturated sodium aluminate solution, method of the present invention can not only be produced single sandy aluminium hydroxide, and can solve kind of the not high shortcoming of branch production sandy aluminium hydroxide rate of decomposition.
Plant branch before the invention reside in employing, add kind of carbon and divide the flow process of planting branch with the back.
Bayer's process production adopts the circulating mother liquor that contains a large amount of free NaOHs to handle bauxite, with stripping wherein aluminum oxide and obtain sodium aluminate solution, therefore must produce aluminium hydroxide with the method for decomposition of crystal seed, simultaneously also make the NaOH in the solution dissociate out, can return after the seed precipitation solution inspissation and join the ore deposit, it then is partly to replenish NaOH for bayer's process that sintering process sodium aluminate solution adopts decomposition of crystal seed.
Sintering process sodium aluminate solution and bayer's process sodium aluminate solution exist difference at aspects such as concentration, degree of supersaturation and foreign matter contents, carry out kind of branch after two kinds of sodium aluminate solutions can mix in integrated process is produced and also can carry out kind of a branch separately, adopt the flow process of carrying out kind of branch separately among the present invention.The timesharing of bayer's process sodium aluminate solution kind adopts the method for producing a part of powdery aluminium hydroxide in the output sandy alumina to improve rate of decomposition, can adopt the flow process of two sections decomposition, produce sandy aluminium hydroxide for first section, produce powdery aluminium hydroxide for two sections, also can adopt general decomposition process, grading, coarse grain partly is a sandy aluminium hydroxide, middle grade is partly returned and made the crystal seed particulate then is powdery aluminium hydroxide partly, (see " light metal " 1983,4, when P12) adopting two sections decomposition process
First section decomposition: 70～75 ℃ of initial temperature, 55～55 ℃ of end temperature, 45～55 hours resolving times.
Second section decomposition: 45～50 ℃ of initial temperature, 35～40 ℃ of end temperature.
Adding kind of carbon, to divide used seed be bayer's process sodium aluminate solution kind branch (preceding kind branch) the powdery aluminium hydroxide that produces, and kind of the carbon branch that adds of the present invention is taked high temperature, slowly decomposes early stage and the method for control stirring intensity.Make powdery aluminium hydroxide be transformed into coarse aluminium hydroxide in the carbon timesharing as crystal seed.Again this carbon branch is produced aluminium hydroxide and also take higher rate of decomposition as sintering process sodium aluminate solution kind branch (back is planted and divided) this kind branch, rate of decomposition 50%, decomposing back gained coarse aluminium hydroxide is exactly sandy aluminium hydroxide.Under normal circumstances, the back is planted and is divided product hydroxide particle-size-44 μ all less than 6%, meets the requirement of sandy alumina production to hydroxide particle-size, does not produce fine-grained aluminum hydroxide.Worsen as working condition, produce partly fine-grained aluminum hydroxide, then product classified after, the independent roasting of fine-grained aluminum hydroxide is a powdery aluminum, selling to the powdery aluminum is the electrolytic aluminium factory user of raw material.At last, whole sandy aluminium hydroxide roastings that front and back two all branch are produced are single sandy alumina product, and the two all minutes rate of decomposition in front and back all can reach 50%.
Preceding granularity and structure of planting the powdery aluminium hydroxide that divides has great effect to adding kind of the granularity and the structure of the aluminium hydroxide of carbon branch product.Add kind of granularity of carbon branch product aluminium hydroxide and structure back granularity and structure of planting the aluminium hydroxide of branch product also had great effect.Under the ordinary production situation, the granularity of preceding kind of branch product powdery aluminium hydroxide can satisfy does to add kind of the requirement of the crystal seed of carbon branch.But when the powdery aluminium hydroxide of preceding kind of branch product was done to add the crystal seed of kind of carbon branch ,-44 μ content % were no more than 50%, and-20 μ content are no more than 20%, because experiment has confirmed to surpass the product that this value is difficult to decomposite release mesh.
Add kind of a carbon branch and can take following technical qualification:
Seed ratio i=0.15～0.05,85 ± 5 ℃ of decomposition temperatures, 5～8 hours resolving times, control carbon divides the decomposition rate at initial stage.Initial stage carbon dioxide feeding amount is not too big.Total rate of decomposition 85～90%, the hydroxide particle-size that is obtained can reach-44 μ＜7%.
Plant branch for the back and can take following technical qualification:
Seed ratio i=1.5 ± 0.5, decomposition temperature: 73 ± 2 ℃ of initial temperature, 50 ± 3 ℃ of end temperature, cooling naturally continuously, 45～60 hours resolving times, rate of decomposition reaches more than 50%.
Be to plant the empirical average result who divides behind the secondary below:
The average decomposition temperature decomposition nut liquid of experiment stoste seed size aluminium hydroxide
Al2O3 α K-44 μ initial temperature end temperature time Al2O3 α K rate of decomposition % aluminium hydroxide
G/l-44 μ % during % ℃ ℃ of fate g/l
8 95.7 1.53 5.78 73 51.8 48 49.2 3.05 49.79 5.35
8 92.8 1.53 5.83 73 48 54 47.5 3.13 50.92 4.68
According to tabular data as seen:
1, average-44 μ of the seed size of Jia Ruing are 5.81%, and through oversintering kind branch, average-44 μ of the granularity of product are 5.01%.Illustrate that the crystal seed that adds is thick, the product that decomposites can be thicker.
2, extended to 54 hours when the resolving time by 48 hours, decompose the end temperature and reduce to 48 ℃ by 52 ℃, rate of decomposition improves about 1%.And product granularity does not attenuate, and proves rate of decomposition 50～51%, fully reliably.
3, under the prerequisite that guarantees product granularity, decomposed 48～54 hours, rate of decomposition reaches 50～51%, and this decomposition rate is very fast, is higher than general kind and divides decomposition rate.As seen back of the present invention is planted the branch advantage and is the rate of decomposition height, and decomposition rate is fast, and the decomposed product granularity is good.
The product of this twice experiment in φ 425 * 5000mm rotary kiln, 1030～1100 ℃ of dynamic roastings, the gained aluminum oxide is a sandy alumina.Data such as following table:
Hydroxide particle-size roasting oxidation aluminium physicals
Title-44 μ % granularity α-equal the alkali of Al2O3 specific surface area abrasion index angle of repose capacity
-44 μ % % m/g % degree g/m %
The back is planted and is divided 4.7～5.4 5.2 20.2 54.9 35.7 3,134 0.39 1.31
The invention has the advantages that the rate of decomposition height, can produce single sandy aluminium hydroxide, the two all minutes rate of decomposition in front and back all can reach 50%, and decomposition rate is fast, also have the carbon of minimizing simultaneously and divide decomposer to scab, and product contains silicon-dioxide and the low advantage of alkali.
The present invention is used for integrated process.The present invention provides a valid approach for handling diaspore type aluminium ore production sandy alumina.
Most preferred embodiment is as follows:
Example one:
Plant before the I and divide: Guizhou Aluminum Factory bayer's process sandy alumina is produced, and plants and divides rate of decomposition 50%.
II adds kind of a carbon branch:
Crystal seed: plant branch before the above-mentioned I and produce powdery aluminium hydroxide ,-44 μ content are 40%.
Decomposer flat pan φ 1000 * 2000mm, multistage paddle stirs, and per minute 20 changes.
Stoste composition: 95 grams per liter Al
2O
3, N
T=110 grams per liters, N
K=91 grams per liters, α
K=1.57.
Seed ratio: 0.15
Furnace gas concentration: 30%CO
2
Carbon divides temperature: 83～90 ℃
Rate of decomposition: the 1st hour be 10%, the 2 hour to be 23.8%, the 3 hour to be 36.6%, the 4 hour to be 49.9%, the 5 hour to be 67%, the 6 hour to be 86.65% to finish.
Gained carbon granularity of seed product accounts for 4.5% for-44 μ.
III, back are planted and are divided:
Experimental installation and scale: one group 9 of seed precipitation tanks, single recess gauge lattice φ 1000 * 2910mm, pneumatic blending, continuous seed component, stock solution flow are 0.25 meter
3/ time.
Stoste: sintering seminal fluid 96.08 grams per liter Al
2O
3,
N
T=107.05 grams per liters, N
K=88.5 grams per liters, α
K=1.52.
Crystal seed: above-mentioned II adds kind of carbon and divides gained aluminium hydroxide, and-44 μ are 4.96%.
Seed ratio: 1.2.
Decomposition temperature: initial temperature is 73.1 ℃, and last temperature is 52.6 ℃, continuously naturally cooling.
Resolving time: 48 hours.
Rate of decomposition: 50.8%
The product hydroxide particle-size :-44 μ are 3.89%.
Example two:
I, preceding kind branch: the Guizhou Aluminum Factory bayer's process is produced sandy aluminium hydroxide, plants and divides rate of decomposition 48%.
II, add kind of a carbon branch:
The decomposer flat pan, φ 1000 * 2000mm, chain type stirs, and per minute 20 changes.
Stoste composition: 98 grams per liter Al
2O
3, N
T=112.4 grams per liters,
N
K=90.7 grams per liters, α
K=1.52.
Crystal seed: plant branch before the above-mentioned I and produce powdery aluminium hydroxide ,-44 μ are 35%.
Seed ratio: 0.4
Furnace gas concentration: 29.4%CO
2
Carbon divides temperature: 84～90.4 ℃.
Rate of decomposition: end in the 1st hour 9.8%, the 2 hour 22%, the 3 hour 42.8%, the 4 hour 67.4%, the 5 hour 87%.
Gained carbon divides the product granularity :-44 μ are 5.9%.
III, back are planted and are divided:
Experimental installation and scale: one group 9 of seed precipitation tanks, single recess gauge lattice φ 1000 * 2910mm, pneumatic blending, continuous seed component, stock solution flow are 0.25 meter
3/ time.
Stoste: sintering seminal fluid 88.77 grams per liter Al
2O
3, N
T=100.47 grams per liters, N
K=85.84 grams per liters, α
K=1.59.
Crystal seed: above-mentioned II adds kind of carbon and divides gained aluminium hydroxide, and-44 μ are 5.9%.
Seed ratio: 1.4.
Decomposition temperature: 73.2 ℃ of initial temperature, last temperature are 48 ℃, continuously naturally cooling.
Resolving time: 54 hours.
Rate of decomposition: 50.62%
The product hydroxide particle-size :-44 μ are 4.28%.
The meaning of each symbol is as follows in the above-mentioned literary composition:
I-seed ratio: add Al in the crystal seed
2O
3Al in content and the solution
2O
3The ratio of content.
α
KThe causticity sodium oxide of-sodium aluminate solution and the molecular ratio of aluminum oxide.
N
KThe concentration g/l of causticity sodium oxide in the-sodium aluminate solution.
N
TThe concentration g/l of total sodium oxide in the-sodium aluminate solution.
Rate of decomposition: represent with the percentage ratio that aluminum oxide branch in the sodium aluminate solution parses.
Planting the branch rate of decomposition is calculated as follows:
η in the formula-kind of branch rate of decomposition, %
α
KaThe molecular ratio of-decomposition stoste.
α
KmThe molecular ratio of-decomposition nut liquid.
Carbon branch rate of decomposition is calculated as follows:
η-carbon divides rate of decomposition in the formula, %
A
aThe alumina concentration of-decomposition stoste, grams per liter.
A
mThe alumina concentration of-decomposition nut liquid, grams per liter.
N
TThe total alkali sodium oxide concentration of-decomposition stoste, grams per liter.
N
TThe total alkali sodium oxide concentration of-decomposition nut liquid, grams per liter.
Claims (1)
1, a kind of from Baeyer--produce the method for sandy alumina the sodium aluminate solution that the sintering integrated process is produced, its characteristics are:
A kind of conventional bayer's process of producing sandy aluminium hydroxide, gained powdery hydroxide particle-size is no more than 50% for-44 μ, and-20 μ are no more than 20%,
As adding the crystal seed that kind of carbon divides;
--adding kind of a carbon branch, is the sintering process seminal fluid of 90～100g/1 with salic concentration, feed carbonic acid gas and decompose, and seed ratio i=0.15～0.5,85 ± 5 ℃ of temperature, the gained hydroxide particle-size is-44 μ＜7%, as planting the crystal seed that divides after the step down;
--the back plant to be divided, and is that the sintering process seminal fluid of 90～100g/1 carries out back and plants and divide with salic concentration, seed ratio i=1.5 ± 0.5, and 73 ± 2 ℃ of initial temperature, warm 50 ± 3 ℃ of end, the sandy aluminium hydroxide that obtains granularity-44 μ＜7% is a product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85105213A CN1011882B (en) | 1985-07-06 | 1985-07-06 | Prodn. sandy aluminium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85105213A CN1011882B (en) | 1985-07-06 | 1985-07-06 | Prodn. sandy aluminium hydroxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85105213A CN85105213A (en) | 1988-11-16 |
| CN1011882B true CN1011882B (en) | 1991-03-06 |
Family
ID=4794330
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85105213A Expired CN1011882B (en) | 1985-07-06 | 1985-07-06 | Prodn. sandy aluminium hydroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1011882B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113037C (en) * | 2000-11-01 | 2003-07-02 | 中国铝业股份有限公司 | Method for preparing super fine aluminium hydroxide |
| CN100339304C (en) * | 2004-05-21 | 2007-09-26 | 山东铝业股份有限公司 | Sand-like alumina producing method for removing periodic subdivision of species fracture |
| CN101607728B (en) * | 2008-06-19 | 2011-04-20 | 北京化工大学 | Method for producing alumina by using sodium bicarbonate to decompose sodium aluminate solution |
| CN105776269B (en) * | 2016-03-24 | 2017-10-17 | 中铝山东新材料有限公司 | Aluminium hydroxide micropowder preparation method and equipment, the aluminium hydroxide micropowder |
| CN107400786A (en) * | 2017-07-04 | 2017-11-28 | 鞍钢集团矿业有限公司 | A kind of method that aluminium is carried from low-grade laterite iron ore |
-
1985
- 1985-07-06 CN CN85105213A patent/CN1011882B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85105213A (en) | 1988-11-16 |
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