CN107879366A - A kind of activation method that aluminum oxide is extracted from flyash - Google Patents

A kind of activation method that aluminum oxide is extracted from flyash Download PDF

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Publication number
CN107879366A
CN107879366A CN201711043300.8A CN201711043300A CN107879366A CN 107879366 A CN107879366 A CN 107879366A CN 201711043300 A CN201711043300 A CN 201711043300A CN 107879366 A CN107879366 A CN 107879366A
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flyash
aluminum oxide
obtains
roasting
temperature
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CN107879366B (en
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郁青春
叶标
杨斌
邓勇
陈秀敏
王飞
徐宝强
刘大春
蒋文龙
李夫
李一夫
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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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
    • C01F7/20Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
    • 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
    • C01F7/20Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
    • C01F7/22Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with halides or halogen acids

Abstract

The present invention relates to a kind of activation method that aluminum oxide is extracted from flyash, belong to aluminum oxide technology field.It is 1 first to cross flyash after ball milling respectively and calcination activation agent after 120 mesh standard sieves according to mass ratio:0.5~4.0 is well mixed, and 0.5~2h of roasting obtains being calcined material under the conditions of then temperature is 750~950 DEG C again;Wherein calcination activation agent is sodium carbonate or sodium chloride and the baking mixed activator of calcium chloride;By obtained roasting material according to liquid-solid ratio be 8~15:It is 1~3mol/L sulfuric acid solutions that 1mL/g, which adds concentration, is 70~90 DEG C of 1~2h of leaching in temperature, separation of solid and liquid obtains aluminum sulfate solution and tailings.This method technique obtains low energy consumption, low cost, the high effect of recovery rate, new method is opened up for the high value added utilization of flyash.

Description

A kind of activation method that aluminum oxide is extracted from flyash
Technical field
The present invention relates to a kind of activation method that aluminum oxide is extracted from flyash, belong to aluminum oxide technology field.
Background technology
Flyash is a kind of solid waste of coal-fired power plant's discharge.China produces substantial amounts of flyash every year, still Utilization rate is relatively low and is that extensive scale utilizes mostly, mainly utilizes in road engineering, stemming operation and architectural engineering.Fine coal Grey chemical composition is based on aluminum oxide and silica, also a small amount of iron oxide and other dissipated metals etc..Extensive style utilizes Huge pressure is not only brought to environment, also wastes the valuable constituent in flyash.This and Resources for construction economizing type, environment are friendly The direction of good type society is inconsistent, so the comprehensive utilization to flyash is increasingly paid attention to now, starts with flyash extraction Aluminum oxide, silica and rare metal, the composite such as synthetic zeolite material and mullite.Aluminum oxide is extracted from flyash Be advantageous to the comprehensive utilization of flyash, there is good Social benefit and economic benefit.
For aluminum oxide in flyash mainly in mullite, mullite property is stably insoluble in soda acid, without handling very It is difficult directly to utilize.Activation process is carried out to flyash, the Al-Si keys destroyed inside mullite, aluminum oxide in flyash is improved and lives Property, be advantageous to the decomposition of mullite and the extraction of aluminum oxide.There is the activating treatment method of many flyash at present, mainly there is machinery Activation, calcination activation, acidleach activation, microwave activation etc..
Mechanical activation can reduce flyash granularity, increase surface of solids product, so as to improve flyash chemism.Tang Yun Deng《Influence of the activation method to alumina leaching in flyash sintered clinker》Light metal, 2009 (4):19-21. experimental studies Show:By controlling other experiment conditions, as mechanical activation degree increases, the dissolution of aluminum oxide takes the lead in subtracting after increasing, and is increasing The dissolution rate of mechanical activation process rear oxidation aluminium brings up to 80.82%.
Calcination activation is current most study, the most ripe activation method of technique.Calcination activation agent mainly has lime stone, alkali Lime, sulfate etc..Zhao's Zhe etc.《Research of the limestone sintering process from flyash extraction aluminum oxide》Metal material and metallurgical work Journey, 2008,36 (2):16-18. carries out limestone sintering process from flyash extraction aluminum oxide experiment, in raw mix formula C/A values For 1.8,1380 DEG C of sintering temperature, under the conditions of the min of soaking time 60, digesting efficiency of alumina is up to more than 79%.Xue Jingen etc. 《Coal ash alkali lime sinter process extracts the research of aluminum oxide》Total utilization of PCA, 1992 (1):20-23. has carried out alkali stone Grey sintering process extracts the research of aluminum oxide from flyash, and when being raw material with desiliconization flyash, calcium ratio is 2.1, and alkali ratio is 0.96, In 1220 DEG C of roasting temperature 30min, aluminum oxide standard dissolution rate is more than 94%.When Lee comes etc.《Prepared by raw material of flyash High purity aluminium oxide》Journal of Chemical Industry and Engineering, 2006,57 (9):2189-2193. experimental studies show ammonium sulfate with granularity D50 at 5 μm Mol ratio is 10, in 400 DEG C of h of roasting temperature 2. 5 in following flyash, then the recovery rate of aluminum oxide is up to 95. 6 %.
Acidleach activation is current activation efficiency highest mode.Mainly there are hydrochloric acid leaching process, concentrated sulfuric acid lixiviation process and solubilization of ammonium fluoride Method.Chang Zhida etc.《The preparation and its application of polymeric aluminum》Liaoning Project Technology University's journal, 2009,28 (s2):100-101. system Standby polymeric aluminum experimental study shows:Flyash is leached after 700 DEG C of calcinings with the hydrochloric acid that concentration is 17 % at 90 DEG C of temperature The volume mass ratio of 3 h, hydrochloric acid and flyash is 4 ml/g, and the extraction rate of aluminium is up to 35 %.It is old towards order etc.《With sulfuric acid from fine coal Aluminum oxide is directly leached in ash》Hydrometallurgy, 2013 (5):309-311. is by experimental study, in liquid-solid ratio 5:1, flyash The extraction time 5h in the initial concentration 3.7mol/L sulfuric acid that temperature is 180 DEG C, leaching rate of alumina 94.16%.Zhao Jianyu etc. 《Research of the solubilization of ammonium fluoride method from flyash extraction aluminum oxide new technology》Inorganic chemicals industry, 2003,35 (4):40-41. is used Aluminum oxide in solubilization of ammonium fluoride method extraction flyash, aluminium leaching rate can reach 97 more than %.
Microwave radiation can improve temperature of reaction system rapidly, promote Al-Si keys to be broken, and reduce reaction activity.Zhao Jianyu Deng《Solubilization of microwave extracts aluminum oxide new technology research from flyash》Inorganic chemicals industry, 2005,37 (2):47-49. using high Warm sintering-microwave radiation joint operation technique, radiates 2-3min, secondary microwave spoke under the W of one-level microwave irradiation power 450 Penetrate under power 720W and radiate 8-10min, the dissolution rate of aluminum oxide is more than 95%.
Several method methods living more than at present all have in laboratory to be studied and obtains good experiment effect, but respective Shortcoming also largely limits its industrialization and used.Price, the recovery rate of the calcination agent of calcination activation be not high, energy consumption is big, The equipment requirement height of acidleach activation, environmental pollution are big, although the high heating technique maximization industrialization of microwave activation recovery rate Difficulty, integrated cost are high.Therefore find that a kind of energy consumption is low, and cost is low, the work method method of the high coal ash lifting aluminum oxide of recovery rate It is highly beneficial.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of extraction aluminum oxide from flyash Activation method.This method technique obtains low energy consumption, low cost, the high effect of recovery rate, is opened for the high value added utilization of flyash Ward off new method.The present invention is achieved through the following technical solutions.
A kind of activation method that aluminum oxide is extracted from flyash, it is comprised the following steps that:
Step 1, first to cross flyash after ball milling respectively and calcination activation agent after 120 mesh standard sieves according to mass ratio be 1:0.5 ~4.0 is well mixed, and 0.5~2h of roasting obtains being calcined material under the conditions of then temperature is 750~950 DEG C again;Wherein roasting is lived Agent is sodium carbonate or sodium chloride and the baking mixed activator of calcium chloride;
Step 2, by the roasting material that step 1 obtains according to liquid-solid ratio be 8~15:It is 1~3mol/L sulfuric acid that 1mL/g, which adds concentration, Solution, it is 70~90 DEG C of 1~2h of leaching in temperature, separation of solid and liquid obtains aluminum sulfate solution and tailings.
The sodium salt of the sodium carbonate or sodium chloride is 1 with calcium chloride mass ratio:1.0~1:9.0.
The beneficial effects of the invention are as follows:
(1)The present invention uses the cheap advantage of compound roasting activator, sodium carbonate or sodium chloride sodium salt activator, also has CaCl2The high feature of activator Al extraction efficiency.
(2)Sintering temperature of the present invention(750-950℃)Compared to limestone sintering process(1300-1400℃)Burnt with soda lime Connection(1200℃)Temperature it is low, energy consumption is small, and cost is low.
(3)The present invention also fits to the alumina content no requirement (NR) in flyash to the low aluminium powder coal ash for not pre-processing desiliconization With.
Embodiment
With reference to embodiment, the invention will be further described.
The flyash of all embodiments of the invention comes from Henan Gongyi thermal power plant, and its chemical composition is as shown in table 1.
The chemical composition of the flyash of table 1(Mass fraction %)
Embodiment 1
This extracts the activation method of aluminum oxide from flyash, and it is comprised the following steps that:
Step 1, flyash after ball milling will be distinguished first(Flyash degree is as shown in table 1)120 are crossed with calcination activation agent After mesh standard sieve according to mass ratio be 1:4.0 is well mixed, and roasting 1.33h is calcined under the conditions of then temperature is 850 DEG C again Material;Wherein calcination activation agent is sodium carbonate and the baking mixed activator of calcium chloride;Sodium carbonate is 1 with calcium chloride mass ratio: 4.0;
Step 2, by the roasting material that step 1 obtains according to liquid-solid ratio be 8:It is 1mol/L sulfuric acid solutions that 1mL/g, which adds concentration, Temperature is 70 DEG C of leaching 1h, and separation of solid and liquid obtains aluminum sulfate solution and tailings.
After the present embodiment, aluminum oxide and dioxide-containing silica in tailings are detected, the recovery rate of aluminum oxide is calculated For 91.83%.Compared with the simple activator only with calcium chloride, cost reduces 1425 yuan/ton, and with only with calcium chloride The recovery rate 91.24% of activator is compared, and recovery rate is more or less the same.
Embodiment 2
This extracts the activation method of aluminum oxide from flyash, and it is comprised the following steps that:
Step 1, flyash after ball milling will be distinguished first(Flyash degree is as shown in table 1)120 are crossed with calcination activation agent After mesh standard sieve according to mass ratio be 1:0.5 is well mixed, and roasting 2h obtains calcining matter under the conditions of then temperature is 750 DEG C again Material;Wherein calcination activation agent is sodium carbonate and the baking mixed activator of calcium chloride;Sodium carbonate is 1 with calcium chloride mass ratio:1;
Step 2, by the roasting material that step 1 obtains according to liquid-solid ratio be 15:It is 3mol/L sulfuric acid solutions that 1mL/g, which adds concentration, It is 90 DEG C of leaching 2h in temperature, separation of solid and liquid obtains aluminum sulfate solution and tailings.
After the present embodiment, aluminum oxide and dioxide-containing silica in tailings are detected, the recovery rate of aluminum oxide is calculated For 88.45%.Compared with the simple activator only with calcium chloride, cost reduces 462 yuan/ton, and with being lived only with calcium chloride The recovery rate 87.8% of agent is compared, and recovery rate is more or less the same.
Embodiment 3
This extracts the activation method of aluminum oxide from flyash, and it is comprised the following steps that:
Step 1, flyash after ball milling will be distinguished first(Flyash degree is as shown in table 1)120 are crossed with calcination activation agent After mesh standard sieve according to mass ratio be 1:2.0 is well mixed, and roasting 0.5h obtains calcining matter under the conditions of then temperature is 950 DEG C again Material;Wherein calcination activation agent is sodium chloride and the baking mixed activator of calcium chloride;Sodium chloride is 1 with calcium chloride mass ratio:9.0;
Step 2, by the roasting material that step 1 obtains according to liquid-solid ratio be 10:It is 2mol/L sulfuric acid solutions that 1mL/g, which adds concentration, It is 80 DEG C of leaching 1.5h in temperature, separation of solid and liquid obtains aluminum sulfate solution and tailings.
After the present embodiment, aluminum oxide and dioxide-containing silica in tailings are detected, the recovery rate of aluminum oxide is calculated For 94.12 %.Compared with the simple activator only with calcium chloride, cost reduces 1128 yuan/ton, and with only with calcium chloride The recovery rate 93.56% of activator is compared, and recovery rate is more or less the same.
The embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party Formula, in those of ordinary skill in the art's possessed knowledge, it can also make on the premise of present inventive concept is not departed from Go out various change.

Claims (2)

1. a kind of activation method that aluminum oxide is extracted from flyash, it is characterised in that comprise the following steps that:
Step 1, first to cross flyash after ball milling respectively and calcination activation agent after 120 mesh standard sieves according to mass ratio be 1:0.5 ~4.0 is well mixed, and 0.5~2h of roasting obtains being calcined material under the conditions of then temperature is 750~950 DEG C again;Wherein roasting is lived Agent is sodium carbonate or sodium chloride and the baking mixed activator of calcium chloride;
Step 2, by the roasting material that step 1 obtains according to liquid-solid ratio be 8~15:It is 1~3mol/L sulfuric acid that 1mL/g, which adds concentration, Solution, it is 70~90 DEG C of 1~2h of leaching in temperature, separation of solid and liquid obtains aluminum sulfate solution and tailings.
2. the activation method according to claim 1 that aluminum oxide is extracted from flyash, it is characterised in that:The sodium carbonate Or the sodium salt of sodium chloride and calcium chloride mass ratio are 1:1.0~1:9.0.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108754127A (en) * 2018-07-12 2018-11-06 昆明理工大学 A method of comprehensive recovery of iron and aluminium from red mud
CN109777960A (en) * 2019-02-25 2019-05-21 河北工程大学 A method of separating and recovering lithium, aluminium from flyash
CN110697750A (en) * 2019-11-19 2020-01-17 中国石油化工股份有限公司 Method for leaching alumina from coal ash generated by gasifying Shell furnace
CN110935717A (en) * 2019-12-16 2020-03-31 金海华 Modification method of high-alumina fly ash
CN111196609A (en) * 2020-03-02 2020-05-26 中南大学 Method for recovering waste carbon material from aluminum electrolysis
CN113061733A (en) * 2021-03-19 2021-07-02 大连理工大学 Method for preparing aluminum-rich leaching solution by using fly ash sintering activation-acid leaching method

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108754127A (en) * 2018-07-12 2018-11-06 昆明理工大学 A method of comprehensive recovery of iron and aluminium from red mud
CN109777960A (en) * 2019-02-25 2019-05-21 河北工程大学 A method of separating and recovering lithium, aluminium from flyash
CN109777960B (en) * 2019-02-25 2020-12-01 河北工程大学 Method for separating and recovering lithium and aluminum from fly ash
CN110697750A (en) * 2019-11-19 2020-01-17 中国石油化工股份有限公司 Method for leaching alumina from coal ash generated by gasifying Shell furnace
CN110935717A (en) * 2019-12-16 2020-03-31 金海华 Modification method of high-alumina fly ash
CN111196609A (en) * 2020-03-02 2020-05-26 中南大学 Method for recovering waste carbon material from aluminum electrolysis
CN111196609B (en) * 2020-03-02 2021-04-13 中南大学 Method for recovering waste carbon material from aluminum electrolysis
CN113061733A (en) * 2021-03-19 2021-07-02 大连理工大学 Method for preparing aluminum-rich leaching solution by using fly ash sintering activation-acid leaching method

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