CN113998719A - Use of leaf filter cake in production of alumina and alumina production method - Google Patents

Use of leaf filter cake in production of alumina and alumina production method Download PDF

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Publication number
CN113998719A
CN113998719A CN202111321516.2A CN202111321516A CN113998719A CN 113998719 A CN113998719 A CN 113998719A CN 202111321516 A CN202111321516 A CN 202111321516A CN 113998719 A CN113998719 A CN 113998719A
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filter cake
slurry
leaf filter
dissolution
bauxite
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廖鹏
吴庆君
郝鹏飞
王宽宽
杨伟
何海军
马志博
高宏涛
张晓龙
张兴
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State Power Investment Group Shanxi Aluminum Industry Co ltd
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State Power Investment Group Shanxi Aluminum Industry Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/04Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/14Aluminium oxide or hydroxide from alkali metal aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/04Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/06Preparation 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

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract

The invention relates to the technical field of alumina production, in particular to application of a leaf filter cake in producing alumina and an alumina production method. The application comprises the following steps: mixing the leaf filter cake with the pre-desilication slurry, and performing dissolution treatment to obtain sodium aluminate dissolution slurry; the pre-desiliconization slurry is obtained by pre-desiliconizing raw ore pulp, wherein the raw ore pulp is obtained by mixing bauxite, circulating mother liquor and lime and then grinding the mixture; wherein the weight ratio of the lime to the bauxite is less than three percent. The scheme of the invention can reduce the addition amount of lime in the production process of alumina, and reduce the cost consumption of raw materials and the emission reduction of red mud.

Description

Use of leaf filter cake in production of alumina and alumina production method
Technical Field
The invention relates to the technical field of alumina production, in particular to application of a leaf filter cake in producing alumina and an alumina production method.
Background
The Chinese bauxite is rich in reserves, and the resources mainly comprise the diaspore ore and have high aluminum (Al2O 350-65%) and high Silicon (SiO)28-15%), low iron composition is complex, and the Al/Si ratio of most ores is A/S<7, which represents about 98% of the total reserves. However, the ore which can meet the requirement of the Bayer process only accounts for about 10 percent of the bauxite resource.
Lime must be added for dissolving out the diaspore ore, and the lime Bayer process dissolving-out technology is generally applied in industry at present. The lime can increase the dissolution speed and dissolution rate, remove elements such as fluorine, phosphorus, vanadium and the like in the solution, convert goethite, eliminate the retardation of sodium titanate on the dissolution of aluminum minerals, and simultaneously has the effects of delaying scarring, purifying impurities and reducing alkali consumption.
At present, in order to eliminate the retardation of titanium minerals in domestic alumina enterprises, the addition of lime is generally over 10 percent. However, the addition of lime also causes a number of adverse effects, namely hydrated pomegranateStone (3 CaO. Al)2O3·xSiO2·yH2O) formation, high losses of alumina. And secondly, the discharge amount of the red mud is increased. Thirdly, calcium carbonate as an impurity causes the caustic loss during the causticization. And the red mud composition is more complex, such as the generation of the calcium iron dealkalized red mud and the more dispersive distribution of various components, thereby increasing the difficulty of separating iron minerals from the red mud.
How to reduce the addition of lime has positive significance for optimizing the production process of alumina.
Disclosure of Invention
In view of the above-mentioned drawbacks and problems of the prior art, it is an object of the present invention to provide a use of a leaf filter cake for the production of alumina and a process for the production of alumina. The scheme is a Bayer process leaf filter cake recycling dissolution process technology, and the leaf filter cake is used as a calcium source to replace part of lime, so that the addition amount of lime in the production process of alumina can be reduced, and the reduction of overall consumption cost and the emission reduction of red mud are realized.
To achieve the above and other related objects, the present invention provides a use of a leaf filter cake in the production of alumina, comprising: mixing the leaf filter cake with the pre-desilication slurry, and performing dissolution treatment to obtain sodium aluminate dissolution slurry; the pre-desiliconization slurry is obtained by pre-desiliconizing raw ore pulp, wherein the raw ore pulp is obtained by mixing bauxite, circulating mother liquor and lime and then grinding the mixture; wherein the weight ratio of the lime to the bauxite is less than three percent.
In one embodiment, the use further comprises: carrying out red mud settling separation, washing and filtering on the dissolved slurry to obtain a crude liquid and red mud; refining the crude liquid by using a leaf filter to obtain refined liquid and a filter cake of the leaf filter; carrying out filter pressing filtration on the filter cake of the leaf filter to obtain a new leaf filter cake and filtrate; and mixing the new leaf filter cake with the pre-desilication slurry, and performing dissolution treatment to obtain the dissolution slurry of the sodium aluminate again.
In one embodiment, the weight ratio of the leaf filter cake to the bauxite is 1% to 4%.
In one embodiment, the mixing bauxite, recycled liquor, and lime includes: 35.17g of bauxite were added per 100mL of circulating mother liquor.
In one embodiment, in the bauxite, Al2O355.84% of SiO2Is 11.55 percent by mass, Fe2O3Is 15.05 percent, TiO2The mass fraction of CaO is 2.32%, and the mass fraction of CaO is 0.19%.
In one example, the circulating mother liquor has a caustic concentration of 252.0g/L, a total caustic concentration of 261.0g/L, an alumina content of 123.7g/L, and a causticization factor of 3.35.
In one embodiment, the temperature of the pre-desilication treatment is 90-100 ℃ and the duration is 6-8 h; the causticization coefficient of the pre-desilication slurry was 1.4.
In one embodiment, the solids content in the leaf filter cake is 346 g/L; wherein, in the leaf filter cake, Al2O3Is 25.69% of SiO2Is 5.7% by mass, Fe2O3Is 3.11 percent of TiO20.9% by mass, 37.37% by mass of CaO, and Na2The mass fraction of O was 2.41%, and the mass fraction of MgO was 0.71%.
In one embodiment, the dissolution temperature of the dissolution treatment is 250-265 ℃, and the dissolution time is 1 h.
The invention also provides an alumina production method, which comprises the following steps: mixing bauxite, circulating mother liquor and lime, and then grinding to obtain raw ore pulp; wherein the weight ratio of lime to bauxite is less than three percent; carrying out pre-desiliconization treatment on the raw ore pulp to obtain pre-desiliconized slurry; mixing the leaf filter cake with the pre-desilication slurry, and carrying out dissolution treatment to obtain the dissolution slurry of sodium aluminate, wherein the dissolution slurry is used for producing alumina.
The application of the leaf filter cake in the production of alumina and the production method of alumina provided by the invention can reduce the addition of lime in the production process of alumina, reduce the consumption of raw material cost and reduce the emission of red mud.
Drawings
FIG. 1 is a flow chart of a process for recycling a filter cake of a leaf filter according to an embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
It should be understood that the structures, ratios, sizes, and the like shown in the drawings are only used for matching the disclosure of the present disclosure, and are not used for limiting the conditions that the present disclosure can be implemented, so that the present disclosure is not limited to the technical essence, and any structural modifications, ratio changes, or size adjustments should still fall within the scope of the present disclosure without affecting the efficacy and the achievable purpose of the present disclosure. In addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not to be construed as a scope of the present invention.
The following reaction can occur by adding lime to the sodium aluminate solution:
3Ca(OH)2+2NaAl(OH)4+aq=3CaO·Al2O3·6H2O+2NaOH+aq
the filter cake of the leaf filter is a filter cake product generated by the leaf filter in the course of refining the crude liquid. Specifically, in the production of alumina, lime is added into the coarse leached ore pulp liquid, then filtration is carried out, the obtained filtrate is settled, then filtration is carried out by using a leaf filter, and a leaf filter cake can be obtained after filtration. The prior art directly discharges the filter cake of the leaf filter into a sedimentation system, and discharges the filter cake together with red mud after washing, so that the utilization rate is not high. Through tests, as shown in Table 1, the content of calcium oxide in the filter cake of the leaf filter is about 37 percent, the content of aluminum oxide is about 26 percent, and the A/S is close to 4.5, so that the leaf filter has further utilization value.
TABLE 1 composition of leaf Filter cake
Figure BDA0003345432440000031
The invention provides a leaf filter cake recycling digestion process technology, which is mainly characterized in that under the same conditions, in the digestion process of bauxite by a Bayer process, a leaf filter cake is taken as a digestion calcium source to replace lime so as to reduce the addition amount of lime in the production process of alumina and realize the reduction of overall consumption cost and the emission reduction of red mud.
The main flow of the dissolution process technology for reusing the leaf filter cake provided by the invention can be shown in fig. 1, and specifically can comprise the following steps.
Mixing bauxite with circulating mother liquor and lime, and grinding to prepare raw ore pulp; wherein, as shown in fig. 1, the bauxite may be diasporic bauxite. The circulating mother liquor has an alkali concentration of 240 to 255g/L and a causticization coefficient (alpha K) of 2.9 to 3.3.
And step two, carrying out pre-desiliconization on the raw ore pulp obtained in the step one to obtain pre-desiliconized slurry. Wherein the pre-desiliconization temperature is 90-100 ℃, and the pre-desiliconization time is 6-8 h.
And step three, fully mixing the pre-desiliconized slurry obtained in the step two with the filter cake of the leaf filter, and then carrying out high-temperature and high-pressure dissolution treatment to obtain dissolved slurry. Wherein the dissolution temperature is 250-265 ℃, and the dissolution time is 1 h.
And step four, diluting and desiliconizing the dissolved slurry obtained in the step three, and then settling, separating, washing and filtering the red mud to obtain crude liquid and red mud.
Step five, refining the crude liquid obtained in the step four through a leaf filter, further removing red mud floating matters in the crude liquid, and obtaining refined liquid and filter cakes of the leaf filter;
and step six, performing filter pressing filtration on the leaf filter cake obtained in the step five to obtain filtrate and the leaf filter cake, and returning the filtrate to the crude liquid tank.
And seventhly, returning part of the leaf filtration filter cake obtained in the sixth step to the third step to be mixed with the pre-desilication slurry, and then implementing the third, fourth, fifth, sixth and seventh steps again to realize the recycling of the leaf filtration filter cake. Wherein the amount of filter cakes returned to the leaf filter in the third step is 2-10 t/h.
According to the amount of filter cakes of the leaf filter in the third step, the corresponding lime amount is calculated, and the lime addition amount is reduced in the original grinding process.
Next, according to the above process flow, different examples were set up to conduct experiments.
Before describing the specific examples, the experimental materials used in the following examples will be described.
The temperature and time of the digestion treatment, the causticization coefficient of the pre-desiliconized slurry, the concentration of the circulating mother liquor, the available calcium content of lime (in mass%), and the solid content of the filter cake of the leaf filter used in the following examples are shown in Table 2.
TABLE 2
Figure BDA0003345432440000041
The compositions of the aluminum ores used in the following examples are shown in table 3. Wherein the amount of each component is expressed by mass percentage.
TABLE 3
Figure BDA0003345432440000042
The analysis of the recycled mother liquor used in the examples below is shown in table 4.
Figure BDA0003345432440000043
The compositional analysis of the leaf filter cake used in each of the examples below is shown in Table 5. Wherein the amount of each component is expressed by mass percentage.
TABLE 5
Figure BDA0003345432440000044
In each of the following examples, 35.17g of aluminum ore was added per 100mL of the circulating mother liquor, and the amount of lime added was 1% by mass of the aluminum ore.
The experimental parameters and indices for each example are shown in table 6.
TABLE 6 Experimental parameters and indices
Figure BDA0003345432440000051
Wherein the elution temperature is the temperature of the elution treatment in the second step. The mass ratio of the leaf filter cake to the aluminum ore is specifically as follows: the mass ratio of the filter cake of the leaf filter used in the third step to the aluminum ore used in the first step. And the dissolution liquid is the dissolution slurry obtained in the third step. And the red mud leaching refers to the red mud obtained in the fourth step. The actual dissolution rate is a ratio obtained by subtracting the aluminum-silicon ratio in the red mud from the aluminum-silicon ratio of the aluminum mineral, and comparing the difference with the aluminum-silicon ratio of the aluminum mineral. The relative dissolution rate refers to a ratio obtained by comparing the actual dissolution rate with the theoretical dissolution rate.
As can be seen from Table 6, the leaching rate of sodium aluminate gradually increases with the increase of leaching temperature under the condition of the same addition ratio of the filter cake. Under the condition of the same dissolution temperature, the A/S in the red mud is gradually reduced along with the increase of the adding proportion of the filter cake of the leaf filter, and the dissolution rate of the sodium aluminate is gradually increased. The filter cake of the leaf filter can be used as a dissolution additive to replace lime, so that the calcium can be recycled.
In summary, the leaf filter cake provided by the invention can replace lime by utilizing the leaching process technology, and under the condition of the same lime addition ratio requirement as the existing process, the addition amount of the lime can be reduced to be within 3% of the dry ore amount of the aluminum ore, so that the aim of reducing the addition of the lime is achieved, the hydrolysis caused after the lime enters a system is reduced, the loss of aluminum oxide is reduced, and the cost consumption of raw materials is reduced.
The invention provides a leaf filter cake recycling and dissolving out process technology, which not only recovers calcium oxide in the leaf filter cake, but also recovers aluminum oxide in the filter cake, belongs to the recycling of waste residues, and realizes the recycling of calcium-containing substances.
The leaf filter cake provided by the invention directly reduces the amount of red mud caused by adding a large amount of lime, promotes the enrichment of valuable minerals in the red mud, creates favorable conditions for the subsequent efficient recovery of alumina and sodium oxide in the red mud, is the most important step in multiple fields of waste resource utilization, energy conservation, emission reduction, safe disposal and the like in the alumina industry, and has great significance for environmental protection.
The leaf filter cake provided by the invention is recycled by using the dissolving-out process technology, has simple flow and obvious economic effect, and has good industrial application prospect.
Therefore, the present invention can effectively overcome the disadvantages of the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. Use of a leaf filter cake in the production of alumina, comprising:
mixing the leaf filter cake with the pre-desilication slurry, and performing dissolution treatment to obtain sodium aluminate dissolution slurry; the pre-desiliconization slurry is obtained by pre-desiliconizing raw ore pulp, wherein the raw ore pulp is obtained by mixing bauxite, circulating mother liquor and lime and then grinding the mixture; wherein the weight ratio of the lime to the bauxite is less than three percent.
2. The use according to claim 1, further comprising:
carrying out red mud settling separation, washing and filtering on the dissolved slurry to obtain a crude liquid and red mud;
refining the crude liquid by using a leaf filter to obtain refined liquid and a filter cake of the leaf filter;
carrying out filter pressing filtration on the filter cake of the leaf filter to obtain a new leaf filter cake and filtrate;
and mixing the new leaf filter cake with the pre-desilication slurry, and performing dissolution treatment to obtain the dissolution slurry of the sodium aluminate again.
3. Use according to claim 1, characterized in that the weight ratio of the leaf filter cake to the bauxite is between 1% and 4%.
4. The use according to claim 1, wherein the mixing of bauxite, recycled liquor and lime comprises: 35.17g of bauxite were added per 100mL of circulating mother liquor.
5. Use according to claim 4, characterized in that in the bauxite, Al2O355.84% of SiO2Is 11.55 percent by mass, Fe2O3Is 15.05 percent, TiO2The mass fraction of CaO is 2.32%, and the mass fraction of CaO is 0.19%.
6. Use according to claim 4, characterized in that in the recycled mother liquor the caustic concentration is 252.0g/L, the total caustic concentration is 261.0g/L, the alumina content is 123.7g/L and the causticisation factor is 3.35.
7. Use according to claim 4, characterized in that the temperature of the pre-desilication treatment is between 90 and 100 ℃ for a duration of between 6 and 8 h; the causticization coefficient of the pre-desilication slurry was 1.4.
8. Use according to claim 4, wherein the solids content in the leaf filter cake is 346 g/L; wherein, in the leaf filter cake, Al2O3Is 25.69% of SiO2Is 5.7% by mass, Fe2O3Is 3.11 percent of TiO20.9% by mass, 37.37% by mass of CaO, and Na2The mass fraction of O was 2.41%, and the mass fraction of MgO was 0.71%.
9. The use according to claim 1, wherein the dissolution temperature of the dissolution treatment is 250 ℃ and 265 ℃ and the dissolution time is 1 h.
10. A method for producing alumina, comprising:
mixing bauxite, circulating mother liquor and lime, and then grinding to obtain raw ore pulp; wherein the weight ratio of lime to bauxite is less than three percent;
carrying out pre-desiliconization treatment on the raw ore pulp to obtain pre-desiliconized slurry;
mixing the leaf filter cake with the pre-desilication slurry, and carrying out dissolution treatment to obtain the dissolution slurry of sodium aluminate, wherein the dissolution slurry is used for producing alumina.
CN202111321516.2A 2021-07-28 2021-11-09 Use of leaf filter cake in production of alumina and alumina production method Pending CN113998719A (en)

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Publication number Priority date Publication date Assignee Title
US4483830A (en) * 1981-09-10 1984-11-20 Comalco Limited Production of alumina
CN1868882A (en) * 2005-05-25 2006-11-29 贵阳铝镁设计研究院 Bauxite grinding technology using evaporating lime treating seed separating raw liquor
CN102674416A (en) * 2012-05-18 2012-09-19 义马煤业集团股份有限公司 Method for producing aluminum oxide-lime blend ores by Bayer process
CN103030161A (en) * 2012-12-21 2013-04-10 中南大学 Application of filter cake of leaf filter
CN105152195A (en) * 2015-08-31 2015-12-16 中国铝业股份有限公司 Treatment method and apparatus for controlled filter cakes in Bayer process for alumina production
CN105905930A (en) * 2016-04-12 2016-08-31 广西华银铝业有限公司 Method for preparing sodium aluminate solution purifying filter aid and utilizing filter cake in alumina production
WO2018233688A1 (en) * 2017-06-23 2018-12-27 东北大学 Method for preparing aluminum hydroxide by treating medium- and low-grade bauxite by using one-step alkali heat process of andradite
CN112158869A (en) * 2020-10-16 2021-01-01 中南大学 Method for dissolving out diasporic bauxite

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4483830A (en) * 1981-09-10 1984-11-20 Comalco Limited Production of alumina
CN1868882A (en) * 2005-05-25 2006-11-29 贵阳铝镁设计研究院 Bauxite grinding technology using evaporating lime treating seed separating raw liquor
CN102674416A (en) * 2012-05-18 2012-09-19 义马煤业集团股份有限公司 Method for producing aluminum oxide-lime blend ores by Bayer process
CN103030161A (en) * 2012-12-21 2013-04-10 中南大学 Application of filter cake of leaf filter
CN105152195A (en) * 2015-08-31 2015-12-16 中国铝业股份有限公司 Treatment method and apparatus for controlled filter cakes in Bayer process for alumina production
CN105905930A (en) * 2016-04-12 2016-08-31 广西华银铝业有限公司 Method for preparing sodium aluminate solution purifying filter aid and utilizing filter cake in alumina production
WO2018233688A1 (en) * 2017-06-23 2018-12-27 东北大学 Method for preparing aluminum hydroxide by treating medium- and low-grade bauxite by using one-step alkali heat process of andradite
CN112158869A (en) * 2020-10-16 2021-01-01 中南大学 Method for dissolving out diasporic bauxite

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