CN110342555A - A method of aluminium oxide is produced containing kaolinic mineral - Google Patents
A method of aluminium oxide is produced containing kaolinic mineral Download PDFInfo
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- CN110342555A CN110342555A CN201910778434.7A CN201910778434A CN110342555A CN 110342555 A CN110342555 A CN 110342555A CN 201910778434 A CN201910778434 A CN 201910778434A CN 110342555 A CN110342555 A CN 110342555A
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- acidleach
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- 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
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
Abstract
The present invention relates to aluminum i ndustry field of engineering technology, a kind of method for specifically disclosing production aluminium oxide containing kaolinic mineral, using soda acid Combined Treatment low-grade bauxite or it is rich in kaolinic gangue, can handle to obtain water purification agent, sodium metasilicate and the high high aluminium material of alumina silica ratio.The present invention is roasted by low-grade bauxite or rich in kaolinic gangue first, activates the aluminium and silicon in kaolinite；Then acidleach is carried out using acid, leaches the aluminium extracted in kaolinite, obtains the raw material that can be used for producing water purification agent and acid leaching residue；Acid leaching residue captures silicon in kaolinite and forms sodium metasilicate, be finally separated by filtration, obtain sodium metasilicate filtrate and alkali soluble filter cake, alkali soluble filter cake are with Al again through alkali soluble desiliconization2O3Based on, alumina silica ratio be greater than 10 high aluminium material, i.e. aluminium concentrate uses as alumina producing raw material.The problems such as present invention solves low-grade bauxite, gangue difficulty utilizes, and resource recovery is low, improves the comprehensive utilization ratio of resource.
Description
Technical field
The present invention relates to aluminum i ndustry field of engineering technology, and in particular to a kind of side of the production aluminium oxide containing kaolinic mineral
Method can handle to obtain the high high aluminium material of alumina silica ratio.
Background technique
Since two thousand eight, for the raw ore grade A/S (alumina silica ratio) of alumina producing between 4.5-5.2, China is every
Nearly 100,000,000 tons of bauxite of year consumption, and only 2,500,000,000 tons of China's bauxite resource amount, and 60% or more the grade of ore is less than
A/S4.5.Bauxite grade is also used the method for being incorporated appropriate high grade ore in A/S3.0 or more at present, makes its equal product
After position reaches about A/S4.0, using finishing.Remaining A/S in 3.0 low-grade bauxites below since alumina silica ratio is low, aluminium oxide
High production cost, so alumina producing enterprise is all reluctant to use, such ore often becomes abandoned mine, slow-witted mine, or in exploitation
Richness is adopted to lose poor and destroyed and abandoned.
With dropping year by year for bauxite grade, processing is carried out to low-grade bauxite, it is comprehensive to carry out efficient resource
It closes and utilizes, to meet the requirement of aluminum i ndustry production, become an important research direction.At present for the comprehensive of low-grade bauxite
It closes and utilizes technique study, be mainly seen in method for floating, method for calcinating, acid processing etc..It is (namely high with diaspore and kaolinite
Ridge soil) based on low-grade bauxite, be a kind of common bauxite in China, producing region include Shanxi with one voice, Xiaoyi, Henan Shan County
Deng.This kind of bauxite, using flotation, lacks effective since the gangue minerals disseminated grain size such as kaolinite is thin, mineralogical property is complicated
Floating agent, product recovery rate are low, at high cost；Using calcining, calcination temperature is high, causes that energy consumption is high, and dissolving out capability is deteriorated, is molten
Low efficiency out；Direct acidleach produces aluminium polychloride, and diaspore therein is difficult to be utilized, and causes a large amount of wastes of resource.
At the same time, gangue is entrained in the rock in coal seam, is the solid mined with discharged during washing coal
Waste is one of maximum industrial waste of China's discharge amount.The kaolinite being rich in gangue is also known as coal series kaolinite.Mesh
Before, China's gangue yield accounts for about the 15%~20% of raw coal output, and accumulation has reached 7,000,000,000 tons, and with annual emissions 1.5
Hundred million tons of speed rapid growth.The chemical component of spoil is more complicated.The main ingredient of gangue is alumino-silicate, wherein containing about
There is 40%~60% or so SiO2, 15%~50% or so Al2O3, there is very big value of exploiting and utilizing, realize gangue
Comprehensive utilization, not only solve to occupy a large amount of soil, moreover it is possible to which the environment for alleviating air, water resource, land resource etc. is asked
Topic.
Therefore, a kind of low cost of researching and designing, efficient process, are handled based on diaspore and kaolinite
Low-grade bauxite and coal series kaolinite, make full use of kaolinite content high and easily-activated feature, to solve its low product
Position, difficult the problem of utilizing, improve the comprehensive utilization ratio of resource, will be of great significance for the aluminum i ndustry production in China.
Summary of the invention
The object of the present invention is to provide a kind of methods of production aluminium oxide containing kaolinic mineral, can handle to obtain high alumina
The aluminium concentrate of silicon ratio, while the raw material and sodium metasilicate that produce for water purification agent can also be obtained.
In order to solve the above technical problems, one technical scheme adopted by the invention is that: one kind is produced containing kaolinic mineral
The method of aluminium oxide, comprising the following steps:
S1: will contain kaolinic mineral calcination activation, and maturing temperature is 400~700 DEG C, calcining time 0.3~2h, described
It is low-grade bauxite or gangue containing kaolinic mineral；The low-grade bauxite is to be with diaspore and kaolinite
The sum of main, diaspore and kaolinic mass percentage content account for the bauxite of 60% or more and alumina silica ratio A/S < 3, institute
Stating gangue is the gangue that kaolinic mass percentage content accounts for 30% or more；
S2: acidleach processing is carried out containing kaolinic mineral to after calcination activation, acid used in acidleach is phosphoric acid, hydrochloric acid, nitre
The mixing of acid, any one or more of sulfuric acid, the liquid-solid ratio of acidleach system for handling are 1:1~6:1, acidleach treatment temperature 20~
110 DEG C, the molten aluminium isolated in kaolinite is soaked in acidleach processing from low-grade bauxite or gangue, filters after acidleach processing,
The pickle liquor containing aluminium is obtained, pickle liquor is water purification agent raw materials for production, and obtained acidleach filter cake is further processed；
S3: the acidleach filter cake is mixed with alkali, and then plus water is made into the reaction paste that liquid-solid ratio is 1:1~4:1, later
Dissolution desiliconization is carried out, 0.3~2h is reacted at 20~110 DEG C, is filtered after completion of the reaction, obtained filtrate is sodium silicate solution,
Resulting filter cake obtains based on aluminium oxide, the high aluminium material of alumina silica ratio A/S > 10 through processing.
Preferably, in step S1, low-grade bauxite or gangue are roasted again after being broken into miberal powder, the mill of miberal powder
Mine fineness is 20%~100% of the total miberal powder weight of miberal powder Zhan less than 0.074mm sieve grade.
Preferably, in step S1, roasting is any one of rotary kiln, shaft furnace, fluidized bed furnace, perpendicular wind furnace with equipment.
Preferably, in step S2, acidleach processing method is one section of acidleach or multistage counter current acid leaching.Multistage counter current acid leaching can be with
Aluminium in kaolinite is kept completely separate out as far as possible.
Preferably, in step S2, sour dosage is the low-grade bauxite or bastard coal after the calcination activation based on concentrated acid
The 30~200% of stone ore powder weight.
Preferably, in step S3, alkali used is the mixing of any one or more of sodium carbonate, sodium hydroxide, potassium hydroxide.
Preferably, in step S3, for the dosage of alkali based on solid base, the weight of alkali is the 30~200% of acidleach filter cake.
The present invention can handle the low-grade bauxite based on diaspore and kaolinite, or containing kaolinite 30% with
On gangue, bauxite or gangue are roasted first, activate the aluminium and silicon in kaolinite；Then acid is carried out using acid
Leaching leaches the aluminium extracted in kaolinite, obtains the raw material that can be used for producing water purification agent and acid leaching residue；Acid leaching residue is de- through alkali soluble again
Silicon, with alkali normal pressure, dosage is moderate, temperature is lower under the conditions of capture kaolinite acidleach after silicon, capture silicon shape in kaolinite
It at sodium metasilicate, is finally separated by filtration, obtains sodium metasilicate filtrate and high-alumina filter cake, alkali soluble filter cake are with Al2O3Based on, aluminium
Silicon uses as alumina producing raw material than the aluminium concentrate greater than 10, can reduce the production cost of alumina industry.Sodium metasilicate filter
Liquid can be used as the raw material of silica gel, adhesive etc..It, can also be using inside gangue when roasting when handling gangue
Heat reduces the dosage of roasting fuel, solves the problems, such as integrated treatment gangue.
The method of kaolinite production aluminium oxide of the present invention, utilizes soda acid joint integrated treatment low-grade bauxite or bastard coal
Stone, easily-activated according to kaolinic aluminium, silicon, using the aluminium in acid dipping separation kaolinite after roasting, acid leaching residue is again in atmospheric low-temperature
It is lower to be reacted with alkali, so that alkali and silicon is formed sodium metasilicate solable matter and carries out desiliconization, it is final to obtain sodium silicate solution and high aluminium silicon ratio
Aluminium concentrate, high aluminium silicon ratio aluminium concentrate is alumina producing raw material.The present invention uses the united method of roasting-acidic leaching with alkaline dissolving
Processing, entire technical process is generated without slag and effluent, economic and environment-friendly.Low-grade bauxite/gangue proposed by the present invention is efficient
Simple using method and process, resource utilization is high, and reagent consumption is low, and investment is small, low in cost, has widened alumina producing source
Channel has good prospects for commercial application to the sustainable development for pushing aluminum i ndustry.The present invention solve low-grade bauxite/
The problems such as gangue difficulty utilizes, the rate of recovery is low, improves the comprehensive utilization ratio of resource, has weight for the aluminum i ndustry production in China
Big meaning.
Detailed description of the invention
Fig. 1 is the flow diagram that the embodiment of the present invention 4 carries out two sections of counterflow leachings.
Specific embodiment
To facilitate the understanding of the present invention, below with reference to embodiment, the present invention will be described in more detail.
Embodiment 1
Taking alumina silica ratio A/S is 3.03 low-grade bauxite, carries out acid and alkali combination method integrated treatment.Low-grade bauxite
Constituent analysis is shown in Table 1.
Table 1
The following steps are included:
1, the low-grade bauxite raw ore is crushed first using crusher, then using ball mill ore grinding to less than
The miberal powder weight accounting of 0.074mm sieve grade is 60%, obtains low-grade bauxite raw ore miberal powder；
2, it is roasted using rotary kiln, 600 DEG C of maturing temperature, roasts 1.5h, kaolinite is activated, is activated
Low-grade bauxite；
3, acidleach is carried out using enamel reaction still, concentrated hydrochloric acid is added, concentrated hydrochloric acid weight is the 100% of mine amount, and water is added to be made into
Liquid-solid ratio is the acidleach system of 3:1,80 DEG C of acidleach temperature, acid-leaching reaction 30min, filtering, from the low-grade bauxite of roasting
Aluminium element is isolated in kaolinite, obtains aluminium oxide 10.46%, the acidleach filtrate of iron oxide 0.63% and acid leaching residue；
4,150% sodium hydrate solid of slag weight is added in acid leaching residue, and the reacting slurry of liquid-solid ratio 1:1 is tuned into water, adjusts
For temperature to 100 DEG C, heat preservation dissolution 1h, filtering obtains the aluminium concentrate of sodium silicate solution and high aluminium silicon ratio through filtering.
The alumina green ore of the present embodiment and obtained aluminium concentrate technical indicator are specifically shown in Table 2.
Table 2
| Sample ID | Yield % | Grade Al2O3% | Grade SiO2% | Alumina silica ratio |
| Aluminium concentrate | 47.5 | 89.23 | 4.03 | 22.14 |
| Low-grade bauxite raw ore | 100.00 | 47.14 | 15.54 | 3.03 |
Embodiment 2
Taking alumina silica ratio is 2.49 low-grade bauxite, carries out acid and alkali combination method integrated treatment.Low-grade bauxite at
Analysis is shown in Table 3.
Table 3
The following steps are included:
1, the low-grade bauxite raw ore is crushed first using crusher, then using ball mill ore grinding to less than
The miberal powder weight accounting of 0.074mm sieve grade is 65%, obtains low-grade bauxite raw ore miberal powder；
2, it is roasted using rotary kiln, 580 DEG C of maturing temperature, roasts 2h, kaolinite is activated, is activated
Low-grade bauxite；
3, acidleach is carried out using enamel reaction still, 100% that concentrated sulfuric acid amount is mine amount is added, adding water to be made into liquid-solid ratio is 3:
1 acidleach system, reacts 60min by 100 DEG C of acidleach temperature, and filtering is isolated from the kaolinite of the low-grade bauxite of roasting
Aluminium element obtains aluminium oxide 10.78%, the acidleach filtrate of iron oxide 0.43% and acid leaching residue；
4, the potassium hydroxide and sodium hydroxide mixed base of 200% 1:1 of slag weight is added in acid leaching residue, is tuned into liquid-solid ratio with water
1:1 reacting slurry, temperature adjustment is to 100 DEG C, heat preservation dissolution 1h, and filtering obtains the aluminium essence of sodium silicate solution and high aluminium silicon ratio through filtering
Mine.
The alumina green ore of the present embodiment and obtained aluminium concentrate technical indicator are specifically shown in Table 4.
Table 4
| Sample ID | Yield % | Grade Al2O3% | Grade SiO2% | Alumina silica ratio |
| Aluminium concentrate | 45.8 | 89.2 | 6.01 | 14.83 |
| Low-grade bauxite raw ore | 100 | 48.34 | 19.41 | 2.49 |
Embodiment 3
Taking alumina silica ratio is 1.85 low-grade bauxite, carries out acid and alkali combination method integrated treatment.Low-grade bauxite at
Analysis is shown in Table 5.
Table 5
The following steps are included:
1, the low-grade bauxite raw ore is crushed first using crusher, then using ball mill ore grinding to less than
The miberal powder weight accounting of 0.074mm sieve grade is 70%, obtains low-grade bauxite raw ore miberal powder；
2, it is roasted using rotary kiln, 660 DEG C of maturing temperature, roasts 2h, kaolinite is activated, is activated
Low-grade bauxite；
3, acidleach is carried out using enamel reaction still, 85% that concentrated sulfuric acid amount is mine amount is added, adding water to be made into liquid-solid ratio is 3:1
Acidleach system, 95 DEG C of acidleach temperature, acid-leaching reaction 60min, filtering, obtain the acid of aluminium oxide 11.38%, iron oxide 0.41%
Lixivium and acid leaching residue；
4, the sodium carbonate and sodium hydroxide mixed base of 150% 1:1 of slag weight is added in acid leaching residue, is tuned into liquid-solid ratio 1 with water:
1 reacting slurry, to 100 DEG C, heat preservation dissolution 1h, filtering obtains the aluminium concentrate of sodium silicate solution and high aluminium silicon ratio through filtering for temperature adjustment.
The alumina green ore of the present embodiment and obtained aluminium concentrate technical indicator are specifically shown in Table 6.
Table 6
| Sample ID | Yield % | Grade Al2O3% | Grade SiO2% | Alumina silica ratio |
| Aluminium concentrate | 42.3 | 75.2 | 6.51 | 11.55 |
| Low-grade bauxite raw ore | 100 | 46.4 | 25.13 | 1.85 |
Embodiment 4
Taking alumina silica ratio is 1.40 low-grade bauxite, carries out acid and alkali combination method integrated treatment.Low-grade bauxite at
Analysis is shown in Table 7.
Table 7
The following steps are included:
1, the low-grade bauxite raw ore is crushed first using crusher, then using rod mill ore grinding to less than
The miberal powder weight accounting of 0.074mm sieve grade is 80%, obtains low-grade bauxite raw ore miberal powder；
2, it is roasted using rotary kiln, 660 DEG C of maturing temperature, roasts 2h, kaolinite is activated, is activated
Low-grade bauxite；
3, acidleach is carried out using enamel reaction still, 100% that concentrated sulfuric acid amount is mine amount is added, adding water to be made into liquid-solid ratio is 3:
1 acidleach system, two sections of counterflow leachings leach flow chart as shown in Figure 1,100 DEG C of temperature, acid-leaching reaction 60min, and filtering obtains
To aluminium oxide 9.37%, the acidleach filtrate of iron oxide 0.45% and acid leaching residue；
4,150% sodium hydroxide of slag weight is added in acid leaching residue, is tuned into liquid-solid ratio 1:1 reacting slurry, temperature adjustment to 100 with water
DEG C, heat preservation dissolution 1h, filtering obtains the aluminium concentrate of sodium silicate solution and high aluminium silicon ratio through filtering.
The alumina green ore of the present embodiment and obtained aluminium concentrate technical indicator are specifically shown in Table 8.
Table 8
| Sample ID | Yield % | Grade Al2O3% | Grade SiO2% | Alumina silica ratio |
| Aluminium concentrate | 35.6 | 72.8 | 6.79 | 10.72 |
| Low-grade bauxite raw ore | 100 | 40.2 | 28.58 | 1.40 |
Embodiment 5
Washing gangue is taken, soda acid Combined Treatment is carried out.The constituent analysis of gangue is shown in Table 9.
Table 9
| Mineral | Anorthite | Illite | Kaolinite | Quartz | Siderite | Rutile |
| Content (%) | 7.3 | 3.7 | 38.6 | 30.71 | 8.5 | 1.42 |
The following steps are included:
1, the gangue raw ore is crushed first using crusher, is then sieved using rod mill ore grinding to less than 0.074mm
The miberal powder weight accounting of net grade is 80%, obtains gangue raw ore miberal powder；
2, it is roasted using rotary kiln, 620 DEG C of maturing temperature, roasts 2h, kaolinite is activated, is activated
Gangue；
3, acidleach is carried out using polytetrafluoro tank, 100% that concentrated hydrochloric acid amount is mine amount is added, adding water to be made into liquid-solid ratio is 3:1
Acidleach system, leached, 100 DEG C of temperature, acid-leaching reaction 45min, filter, obtain aluminium oxide 10.29%, iron oxide
0.37% acidleach filtrate and acid leaching residue；
4,170% sodium hydroxide of slag weight is added in acid leaching residue, is tuned into liquid-solid ratio 2:1 reacting slurry, temperature adjustment to 100 with water
DEG C, heat preservation dissolution 1h, filtering obtains the aluminium concentrate of sodium silicate solution and high aluminium silicon ratio through filtering.
The gangue and aluminium concentrate technical indicator of the present embodiment are specifically shown in Table 10.
Table 10
It should be noted that unless otherwise defined, all technical and scientific terms used in this specification with belong to
The normally understood meaning of those skilled in the art of the invention is identical.Used term in the description of the invention
It is the purpose in order to describe specific embodiment, is not intended to the limitation present invention.
Claims (7)
1. a kind of method of the production aluminium oxide containing kaolinic mineral, it is characterised in that: the following steps are included:
S1: will contain kaolinic mineral calcination activation, and maturing temperature is 400~700 DEG C, calcining time 0.3~2h, described containing height
The mineral of ridge stone are low-grade bauxite or gangue；The low-grade bauxite be based on diaspore and kaolinite,
The sum of diaspore and kaolinic mass percentage content account for the bauxite of 60% or more and alumina silica ratio A/S < 3, the coal
Spoil is the gangue that kaolinic mass percentage content accounts for 30% or more；
S2: acidleach processing is carried out containing kaolinic mineral to after calcination activation, acid used in acidleach is phosphoric acid, hydrochloric acid, nitric acid, sulphur
The mixing of any one or more of acid, the liquid-solid ratio of acidleach system for handling are 1:1~6:1, acidleach treatment temperature 20~110
DEG C, the molten aluminium isolated in kaolinite is soaked in acidleach processing from low-grade bauxite or gangue, filters, obtains after acidleach processing
Pickle liquor containing aluminium, pickle liquor are water purification agent raw materials for production, and obtained acidleach filter cake is further processed；
S3: the acidleach filter cake is mixed with alkali, and then plus water is made into the reaction paste that liquid-solid ratio is 1:1~4:1, is carried out later
Desiliconization is dissolved out, 0.3~2h is reacted at 20~110 DEG C, is filtered after completion of the reaction, obtained filtrate is sodium silicate solution, gained
Filter cake through processing obtain based on aluminium oxide, the high aluminium material of alumina silica ratio A/S > 10.
2. the method for the production aluminium oxide according to claim 1 containing kaolinic mineral, it is characterised in that: in step S1,
Low-grade bauxite or gangue are roasted again after being broken into miberal powder, and the grinding fineness of miberal powder is less than 0.074mm sieve
The 20%~100% of the total miberal powder weight of the miberal powder Zhan of grade.
3. the method for the production aluminium oxide according to claim 2 containing kaolinic mineral, it is characterised in that: in step S1,
Roasting is any one of rotary kiln, shaft furnace, fluidized bed furnace, perpendicular wind furnace with equipment.
4. the method for the production aluminium oxide according to claim 3 containing kaolinic mineral, it is characterised in that: in step S2,
Acidleach processing method is one section of acidleach or multistage counter current acid leaching.
5. the method for the production aluminium oxide according to claim 4 containing kaolinic mineral, it is characterised in that: in step S2,
The dosage of acid is 30~200% of low-grade bauxite or gangue miberal powder weight after the calcination activation based on concentrated acid.
6. the method for the production aluminium oxide according to claim 5 containing kaolinic mineral, it is characterised in that: in step S3,
Alkali used is the mixing of any one or more of sodium carbonate, sodium hydroxide, potassium hydroxide.
7. the method for the production aluminium oxide according to claim 6 containing kaolinic mineral, it is characterised in that: in step S3,
For the dosage of alkali based on solid base, the weight of alkali is the 30~200% of acidleach filter cake.
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| CN111268686A (en) * | 2020-02-08 | 2020-06-12 | 昆明理工大学 | Method for preparing water glass from silicate minerals and water glass |
| CN112875736A (en) * | 2021-03-11 | 2021-06-01 | 太原理工大学 | Method for co-producing adsorption material and aluminum oxide by using tail coal |
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| CN112875736A (en) * | 2021-03-11 | 2021-06-01 | 太原理工大学 | Method for co-producing adsorption material and aluminum oxide by using tail coal |
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