CN109650420B - Method for producing sandy alumina by using Bayer process in one section - Google Patents
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- CN109650420B CN109650420B CN201910118430.6A CN201910118430A CN109650420B CN 109650420 B CN109650420 B CN 109650420B CN 201910118430 A CN201910118430 A CN 201910118430A CN 109650420 B CN109650420 B CN 109650420B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
- C01F7/0666—Process control or regulation
Abstract
The present invention regulates the decomposing condition of crystal seed and active additive according to the accurate prediction of fine grain content and its change trend in crystal seed, and changes the agglomeration quantity of fine grain in crystal seed to stabilize the grain size of crystal seed to 45 micronsIn the required range of 10-20%, selecting the nucleation frequency f3.55 of the seed crystal and the content of the granularity of-14 μm as the reference standard for measuring the amount of the fine particles, and setting the control range of the nucleation frequency f3.55 of the seed crystal to be 0.56-1.11 multiplied by 105(ii) a The content control range of the seed crystal granularity of-14 mu m is set to be 0.3-0.6 percent; sampling and detecting are carried out for one sample application every eight hours at a frequency, and the crystal seed decomposition conditions and the active additives are adjusted according to the standard range, so that the content of the crystal seed with the granularity of-45 mu m in a section of Bayer process seed separation is 10-20%, and the decomposition rate is more than or equal to 50%. The invention provides a method for producing sandy alumina by a Bayer process, which is suitable for the bauxite resource characteristics and the production condition characteristics of China, and has the advantages of simple process flow, convenient operation, low energy consumption and low cost.
Description
Technical Field
The invention relates to the field of chemical product preparation, in particular to a process for producing alumina by taking bauxite as a raw material, and particularly relates to a method for producing sandy alumina by Bayer process seed precipitation.
Background
There are various methods for extracting alumina from bauxite, for example: bayer process, soda lime sintering process, bayer-sintering combination process, etc. The bayer process has been the major method for producing alumina, with yields of about 95% of the total alumina production worldwide. The Bayer process has the advantages that: simple flow, low investment and energy consumption, and the lowest energy consumption of about 3 multiplied by 106 kilocalories per ton of alumina. The Bayer process of producing alumina is divided into Mei-Al process and Fa-Al process, the Mei-Al process is also called two-stage process, which is a mechanism of effectively utilizing agglomeration and crystal growth, and generally adopts the conditions of higher decomposition initial temperature and lower seed crystal ratio. The aluminum method is also called a section method, the decomposition process is mainly a crystal growth mechanism, and the method is under the conditions of lower decomposition temperature and higher seed crystal ratio. At present, the alumina crystal seed decomposition process in China mostly adopts a section of Bayer process with low energy consumption and low cost, but the alumina production technology has great limitation when being used in the alumina production process taking diasporic bauxite as raw material in China: in the existing Bayer process seed crystal decomposition in China, high-concentration sodium aluminate solution is added into aluminum hydroxide seed crystals, decomposition is carried out for 40-60 hours at the decomposition initial temperature of about 60 ℃, the final temperature reaches 45-50 ℃, and the produced aluminum hydroxide and aluminum oxide products have low strength and fine granularity and cannot meet the requirements of high-quality sandy aluminum oxide.
The patent with application number 200610127175.4 adopts two-stage Bayer process seed precipitation production process combining two kinds of concentrated semen, namely high-temperature low-concentration agglomeration and low-temperature high-concentration growth to produce high-strength alumina, and solves the defects that the relative supersaturation of the high-concentration semen alumina of the patent with application number 200410049746 is low, the agglomeration driving force is small, the agglomeration effect is not obvious, the content of-20 microns in the product can not meet the requirements of the modern electrolysis process, and the high agglomeration effect of the semen concentration of the semen separation agglomeration stage in the patent with application number 200410100973 is stopped, but two kinds of semen concentrations and the two-stage seed precipitation process have a prominent fatal problem: the process is complex, the energy consumption is high and the cost is high. Two aspects are embodied: 1) the fine seeds and the coarse seeds are decomposed by two semen concentrations and a two-stage method, and two sets of corresponding equipment and two flows are required to be prepared respectively, so that the equipment investment is large, the process parameters are large, and the operation control difficulty is increased; 2) compared with the seed crystal decomposition process by the one-stage method, the seed crystal decomposition process by the two-stage method has the advantages of more operation equipment, high energy consumption, higher decomposition temperature control, short decomposition time, low decomposition rate, high consumption, low yield and high processing cost. The original AB group seed crystal decomposition system of 70 ten thousand tons of alumina production lines of Henan division of aluminum, Henan, China, adopts a two-stage method to produce sandy alumina, and because the operation cost is high, the operation is only 4 years, and the two-stage method is changed into the one-stage method in 2010, the production cost and pressure of the alumina are increased along with the aggravation of the alumina market competition, and the two-stage method seed crystal decomposition process has little popularization significance and is not widely applied.
Disclosure of Invention
The invention aims to overcome the defects of complex flow, high energy consumption and high cost in the prior two-stage alumina production technology, and provides a method for producing sandy alumina by a Bayer process, which is suitable for the bauxite resource characteristics and the production condition characteristics in China, and has the advantages of simple process flow, convenient operation, low energy consumption and low cost.
To achieve the above object, the present invention adopts the techniqueThe scheme is as follows: a method for producing sandy alumina by a one-stage Bayer process seed separation method comprises the steps of adjusting seed crystal decomposition conditions and active additives according to accurate prediction of content and variation trend of fine particles in seed crystals, changing agglomeration quantity of the fine particles in the seed crystals to enable the content of the-45 mu m particle size of the seed crystals to be stabilized within a required range of 10-20%, selecting the content of the-14 mu m particle size of the seed crystals with nucleation frequency f3.55 as a reference standard for measuring the amount of fine particles, and respectively determining standard control ranges of the fine particles: the particle counter has a threshold value of 1.5 μm when detecting with a small-hole tube of 50 μm, and a seed crystal nucleation frequency f3.55 control range of 0.56-1.11 × 105(ii) a When the particle counting instrument uses a small-hole tube with 280 mu m for detection, the threshold value is set to be 9.5 mu m, the content control range of the seed crystal granularity of 14 mu m is set to be 0.3-0.6 percent, and the seed crystal nucleation frequency f3.55 and the seed crystal granularity of 14 mu m are selected as seed crystal regulation indexes;
the sampling detection frequency is one sample per eight hours, and the method for adjusting the seed crystal decomposition conditions and the active additives according to the standard range is as follows: when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of the seed crystal of-14 mu m fluctuate within the given standard range, various decomposition conditions and the addition amount of the crystallization auxiliary agent are kept unchanged; the nucleation frequency f3.55 of the seed crystal and the content of the grain size of the seed crystal of-14 mu m are both in the standard ranges given above, but the seed crystal tends to rise continuously for 48 hours, and the addition amount of the crystallization auxiliary agent is adjusted up to 5 ppm; the nucleation frequency f3.55 of the seed crystal and the content of the-14 mu m particle size of the seed crystal exceed the upper limit values of the given standard ranges and still show an ascending trend, the addition amount of the crystallization auxiliary agent is increased by 5-10 ppm, and the temperature of the first tank of the decomposition tank is increased by 1-2 ℃; the nucleation frequency f3.55 of the seed crystal and the content of the-14 mu m particle size of the seed crystal exceed the upper limit value of the given standard, but the seed crystal continuously decreases in 48 hours, and the temperature of the first tank of the decomposition tank is reduced by 0.5-1 ℃; when the nucleation frequency f3.55 and the granularity of-14 mu m of the seed crystal are both reduced to the upper limit value of the given standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 5 ppm; when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of-14 mu m of the seed crystal are both reduced to the central value of the given standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 5 ppm; when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of the seed crystal of-14 mu m are both reduced to the lower limit value of the given standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 10 ppm; when the nucleation frequency f3.55 and the grain size of the seed crystal of-14 microns are lower than the lower limit value of the given standard range and still show a descending trend, stopping adding the crystallization auxiliary agent, and slowly reducing the temperature of the first tank of the decomposition tank by 0.5-1 ℃; the nucleation frequency f3.55 of the seed crystal and the grain size of-14 microns of the seed crystal are lower than the lower limit value of the given standard range, the change trend of the two indexes is changed from reduction to stabilization, and the addition of the crystallization aid is recovered or the addition of the crystallization aid is slightly increased to 5 ppm; when the nucleation frequency f3.55 and the grain size-14 microns of the seed crystal are increased to the lower limit of the required standard range, the addition amount of the crystallization auxiliary agent is increased by 5-10 ppm to slow the increasing speed of the nucleation frequency f3.55 and the grain size-14 microns of the seed crystal until the content fluctuates in the required standard range.
Seed crystal decomposition control conditions: the Nk concentration of the high-concentration sodium aluminate concentrate is more than or equal to 155g/L, the caustic ratio is less than or equal to 1.55, the NcNt of the concentrate is less than or equal to 15%, the temperature of a first decomposition tank is 58-62 ℃, the temperature of a tail decomposition tank is 45-50 ℃, the solid content of the decomposition tank is 500-1000 g/L, the decomposition time is 40-50 h, the content of the seed crystal with the granularity of-45 mu m in a Bayer process in one section is 10-20%, and the decomposition rate is more than or equal to 50% in the control.
The technical scheme of the invention has the following positive effects: the method of the invention provides artificial intervention and regulation of the agglomeration amount of fine particles of the seed crystal under the low temperature condition on the basis of patent 200410049746, and stabilizes the granularity of the seed crystal of a section of Bayer process. Detecting the number of fine particles less than or equal to 15 microns in the seed crystal by using a special particle counting instrument, establishing several fine particle index control standard ranges in the seed crystal, guiding and adjusting certain decomposition conditions and changing the addition amount of an active crystallization aid according to the content and the variation trend of the fine particles in the seed crystal particle size, manually intervening the agglomeration degree of the fine particles, and controlling the content of the fine particles in the standard range by changing the agglomeration adjustment of the fine particles so as to realize the stable control of the seed crystal particle size to 45 microns. In the production of alumina, in order to obtain a sand-shaped alumina product with stable granularity index, the granularity of seed crystal must be stably controlled. The content of the seed crystal with the granularity of-45 mu m is determined by the content control of the fine particles at the early stage, the content of the fine particles in the seed crystal is controlled, the content of the seed crystal with the granularity of-45 mu m at the later stage is better controlled, and the requirement of producing the sandy alumina product with stable granularity is met.
Detailed Description
The technical solution of the present invention will be further illustrated and described with reference to specific examples.
A method for producing sandy alumina by Bayer seed production in one section adjusts the decomposition condition of seed crystals and active additives according to the accurate prediction of the content and the variation trend of fine particles in the seed crystals, changes the agglomeration amount of the fine particles in the seed crystals to ensure that the content of the-45 mu m particle size of the seed crystals is stabilized within the required range of 10-20 percent, selects the content of the f3.55 nucleation frequency and the-14 mu m particle size of the seed crystals as reference standards for measuring the amount of fine particles, and respectively establishes the standard control ranges thereof: the particle counter has a threshold value of 1.5 μm when detecting with a small-hole tube of 50 μm, and a seed crystal nucleation frequency f3.55 control range of 0.56-1.11 × 105(ii) a The threshold value of the particle counting instrument is set to 9.5 mu m when the particle counting instrument uses a small-hole tube with the size of 280 mu m for detection, the content control range of the seed crystal granularity of 14 mu m is set to 0.3-0.6 percent, and the seed crystal nucleation frequency f3.55 and the content of the seed crystal granularity of 14 mu m are selected as seed crystal regulation indexes.
The control range of the seed crystal particle size of-45 μm is set according to: according to the requirement that the content of metallurgical grade sandy alumina is less than or equal to 18 percent of-45 mu m, and the difference value between the content of the general flat disc aluminum hydride is less than or equal to 8 percent and the content of the product alumina is less than or equal to 8 percent, the control range of the content of the flat disc aluminum hydride is determined to be less than or equal to 10 percent, then the particle size grading reduction coefficient of a hydraulic cyclone is 2.0, the content of the decomposed seed crystal of-45 mu m is determined to be less than or equal to 20 percent, and the control range of the particle size of the seed crystal is not too coarse for ensuring the index of the decomposition rate, so the control range of the content of the decomposed seed crystal of.
The control range of the seed crystal granularity of-14 μm is set according to the following steps: according to the direct proportion relationship between the solid particle mass and the volume, the control range of the seed crystal particle size-14 μm content can be calculated from the control range of the seed crystal particle size-45 μm content 10-20%: upper limit = 20%/(45 ÷ 14)3= 0.60%; lower limit = 10%/(45 ÷ 14)3= 0.30%. Therefore, the content control range of the grain size of the decomposition seed crystal of-14 mu m is set to be 0.3-0.6%.
The nucleation frequency f3.55 of the seed crystal refers to the average step size of 0.1 mu m in the interval of 2.62 mu m-3.55 mu m of the seed crystal particle size in 1g of seed crystal sample. The specific weight of the seed crystal aluminum hydroxide is 2.42g/cm3。
The control range of the nucleation frequency f3.55 of the seed crystal is set according to the following steps: and similarly, according to the proportional relation between the mass and the volume of the solid particles, the control range of the particle content in the interval of 2.62-3.55 mu m of the seed crystal particle size can be calculated from the control range of 10-20% of the seed crystal particle size-45 mu m: upper limit = 20%/((45 ÷ 3.55)3－（45÷2.62）3) = 0.00587%; lower limit = 10%/((45 ÷ 3.55)3－（45÷2.62）3) = 0.00294%. The nucleation frequency of the seed crystal is f3.55 control range: upper limit =0.00587% × 1 ÷ (2.42 × 4/3 × 3.14 × (3.55/20000)3）×0.1÷(3.55-2.62)=1.11×105(ii) a Lower limit =0.00294% × 1 ÷ (2.42 × 4/3 × 3.14 × (3.55/20000)3）×0.1÷(3.55-2.62)=0.56×105. Therefore, the nucleation frequency f3.55 of the decomposition seed crystal is controlled to be 0.56-1.11 × 105。
The method for adjusting the seed crystal decomposition conditions and the active additive according to the above standard ranges is as follows:
when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of the seed crystal of-14 mu m fluctuate within the required standard range, various decomposition conditions and the addition amount of the crystallization auxiliary agent are kept unchanged; the nucleation frequency f3.55 of the seed crystal and the content of the grain size of the seed crystal of-14 mu m are both in the standard ranges given above, but the seed crystal tends to rise continuously for 48 hours, and the addition amount of the crystallization auxiliary agent is adjusted up to 5 ppm; the nucleation frequency f3.55 and the grain size of the seed crystal of-14 microns exceed the given standards and still show an ascending trend, the addition amount of the crystallization auxiliary agent is adjusted up to 5-10 ppm, the maximum addition amount is adjusted up to 30ppm, and the temperature of the first tank of the decomposition tank is adjusted up to 1-2 ℃; the nucleation frequency f3.55 and the grain size of the seed crystal of-14 microns are higher than the given standards, but the seed crystal shows a descending trend after continuous 48 hours, and the temperature of the first tank of the decomposition tank is reduced by 0.5-1 ℃; when the nucleation frequency f3.55 and the granularity of-14 mu m of the seed crystal are both reduced to the upper limit value of the given standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 5 ppm; when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of-14 mu m of the seed crystal are both reduced to the central value of the given standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 5 ppm; when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of the seed crystal of-14 mu m are both reduced to the lower limit value of the given standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 10 ppm; when the nucleation frequency f3.55 and the grain size of the seed crystal of-14 microns are lower than the given standard range and still show a descending trend, stopping adding the crystallization auxiliary agent, and slowly reducing the temperature of the first tank of the decomposition tank by 0.5-1 ℃; the nucleation frequency f3.55 of the seed crystal and the grain size of-14 microns of the seed crystal are lower than the given standard range, the change trend of the two indexes is changed from reduction to stabilization, and the addition of the crystallization aid is restored or the addition of the crystallization aid is slightly increased to 5 ppm; when the nucleation frequency f3.55 and the grain size-14 microns of the seed crystal are increased to the lower limit of the required standard range, the addition amount of the crystallization auxiliary agent is increased by 5-10 ppm to slow the increasing speed of the nucleation frequency f3.55 and the grain size-14 microns of the seed crystal until the content fluctuates in the required standard range. If the nucleation frequency f3.55 of the seed crystal and the content of the seed crystal with the particle size of-14 mu m can be stably regulated and controlled, the particle size of the seed crystal with the particle size of-45 mu m at the later stage can be stably controlled, and the decomposed seed crystal slurry is classified according to the conventional method and then washed to filter out an aluminum hydroxide product, or is roasted to produce a qualified sandy aluminum oxide product.
Seed crystal particle size detection analyzer: beckmann Coulter counter analyzer Multisizer3, pore tubes 50 μm and 280 μm. The control range of the seed crystal nucleation f3.55 is required to be 0.56-1.11 multiplied by 105The grain size content of 14 mu m is required to be controlled within the range of 0.3-0.6%.
In a certain component decomposing tank, the concentration of the semen Nk is 1.60-165 g/L, the concentration of the semen ak is 0.45-1.5, the concentration of the semen NcNt is 14-14.5%, the temperature of the first tank of the decomposing tank is 60-62 ℃, the solid content of the decomposing tank is 500-700 g/L, the decomposing time is 40-43 hours, the index of the decomposing rate is controlled at 49-51%, and the average value is 50.12% from 3 months 1 to 12 months 31 days in 2017. The practical control range of the seed crystal nucleation f3.55 is 0.6-1.0 multiplied by 105Average of 0.73X 105The control range of 14 mu m particle size content is 0.3-0.55 percent, the average is 0.50 percent, the control range of seed crystal-45 mu m particle size content is 13-18 percent, and the average is 16.7 percent; the control range of the-45 mu m particle size content of the aluminum hydroxide product is 4-10 percent, and the average particle size is 8.5 percent; the content control range of the granularity of the alumina product, namely-45 mu m, is 10-17%, and 15% on average.
Claims (2)
1. A method for producing sandy alumina by a one-stage Bayer process seed separation is characterized in that: the method comprises the steps of adjusting seed crystal decomposition conditions and active additives according to accurate prediction of the content and the variation trend of fine particles in seed crystals, changing the agglomeration amount of the fine particles in the seed crystals to enable the content of-45 mu m of the particle size of the seed crystals to be stabilized within the required range of 10-20%, selecting the nucleation frequency f3.55 and the content of-14 mu m of the seed crystals as reference standards for measuring the amount of the fine particles, and respectively determining the standard control ranges: the particle counter has a threshold value of 1.5 μm when detecting with a small-hole tube of 50 μm, and a seed crystal nucleation frequency f3.55 control range of 0.56-1.11 × 105(ii) a When the particle counting instrument uses a small-hole tube with 280 mu m for detection, the threshold value is set to be 9.5 mu m, the content control range of the seed crystal granularity of 14 mu m is set to be 0.3-0.6 percent, and the seed crystal nucleation frequency f3.55 and the seed crystal granularity of 14 mu m are selected as seed crystal regulation indexes;
the sampling detection frequency is one sample per eight hours, and the method for adjusting the seed crystal decomposition conditions and the active additives according to the standard range is as follows: when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of the seed crystal of-14 mu m fluctuate within the standard range, various decomposition conditions and the addition amount of the crystallization auxiliary agent are kept unchanged; the nucleation frequency f3.55 of the seed crystal and the grain size of the seed crystal of-14 mu m are both in the standard ranges, but the seed crystal tends to rise continuously for 48 hours, and the addition amount of the crystallization auxiliary agent is adjusted up to 5 ppm; the nucleation frequency f3.55 of the seed crystal and the content of the-14 mu m particle size of the seed crystal exceed the upper limit value of the standard range and still show an ascending trend, the addition amount of the crystallization auxiliary agent is increased by 5-10 ppm, and the temperature of the first tank of the decomposition tank is increased by 1-2 ℃; the nucleation frequency f3.55 of the seed crystal and the content of the grain size of-14 microns of the seed crystal exceed the upper limit value of the standard, but show a descending trend after continuous 48 hours, and the temperature of the first tank of the decomposition tank is reduced by 0.5-1 ℃; when the nucleation frequency f3.55 and the granularity of-14 mu m of the seed crystal are both reduced to the upper limit value of the standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 5 ppm; when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of-14 mu m of the seed crystal are both reduced to the central value of the standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 5 ppm; when the nucleation frequency f3.55 of the seed crystal and the content of the granularity of the seed crystal of-14 mu m are both reduced to the lower limit value of the standard range and still show a descending trend, the addition amount of the crystallization auxiliary agent is reduced by 10 ppm; when the nucleation frequency f3.55 and the grain size of the seed crystal of-14 microns are lower than the lower limit value of the standard range and still show a descending trend, stopping adding the crystallization auxiliary agent, and slowly reducing the temperature of the first tank of the decomposition tank by 0.5-1 ℃; the nucleation frequency f3.55 of the seed crystal and the grain size of-14 microns of the seed crystal are lower than the lower limit value of the standard range, the change trend of the two indexes is changed from reduction to stabilization, and the addition of the crystallization aid is restored or the addition of the crystallization aid is slightly increased to 5 ppm; when the nucleation frequency f3.55 and the grain size-14 microns of the seed crystal are increased to the lower limit of the required standard range, the addition amount of the crystallization auxiliary agent is increased by 5-10 ppm to slow the increasing speed of the nucleation frequency f3.55 and the grain size-14 microns of the seed crystal until the content fluctuates in the required standard range.
2. The method of producing sandy alumina in a section of the bayer process according to claim 1, wherein: seed crystal decomposition control conditions: the Nk concentration of the high-concentration sodium aluminate concentrate is more than or equal to 155g/L, the caustic ratio is less than or equal to 1.55, the NcNt of the concentrate is less than or equal to 15%, the temperature of a first decomposition tank is 58-62 ℃, the temperature of a tail decomposition tank is 45-50 ℃, the solid content of the decomposition tank is 500-1000 g/L, the decomposition time is 40-50 h, the content of the seed crystal with the granularity of-45 mu m in a Bayer process in one section is 10-20%, and the decomposition rate is more than or equal to 50% in the control.
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