CN103482707A - Fractional precipitation method for extraction of aluminum, silicon, iron and calcium elements in fly ash - Google Patents
Fractional precipitation method for extraction of aluminum, silicon, iron and calcium elements in fly ash Download PDFInfo
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Abstract
The invention discloses a fractional precipitation method for extraction of aluminum, silicon, iron and calcium elements in fly ash, and the method comprises (1) the fly ash activated by roasting is leached by hydrochloric acid, and then filtered to obtain filter residue and filtrate, and the filter residue is further processed to obtain white carbon black; (2) the pH value of the filtrate obtained by the step (1) is adjusted to 1.5 - 3.5, then filter residue and filtrate are obtained by precipitation and filtering, and an iron compound is obtained by washing and drying of the filter residue; (3) the pH value of the filtrate obtained by the step (2) is adjusted to 3.8 - 5.2, then filter residue and filtrate are obtained by precipitation and filtering, and aluminum hydroxide is obtained by washing and drying of the filter residue, and then metallurgical grade alumina is obtained by further calcinations; and (4) calcium chloride dihydrate is obtained by evaporating of the filtrate obtained by the step (3), and anhydrous calcium chloride is obtained by further calcinations. Through use of the method, fractional extraction of the aluminum, silicon, iron and calcium elements in the fly ash can be realized, and the extraction rates are more than 70%. At the same time, the method is simple in process and low in cost.
Description
Technical field
The invention belongs to the meticulous higher value application of flyash field, particularly a kind of aluminium that extracts, silicon, the method for the fractional precipitation of iron and calcium from flyash.
Background technology
In recent years, the coal electricity industry of China brought the sharply increase of solid waste coal ash quantity discharged when developing rapidly, by 2007, the annual emissions of China's flyash is over 200,000,000 tons, and still increasing year by year, the accumulative total volume of cargo in storage surpasses 2,500,000,000 tons, floor space 50,000 hm
2above.The flyash of a large amount of discharges had both taken a large amount of soils, and again to soil, water resources and air cause severe contamination.Therefore, the comprehensive utilization of flyash has become the important topic that China researchs and solves for many years.
At present, flyash is being built work, and a plurality of fields such as building are applied, although large usage quantity, its digestion amount is unable to catch up with the growth of quantity discharged far away, and belongs to low value-added, the extensive style utilization of low technical content.On the other hand, contain abundant aluminium in flyash, silicon, the useful element such as iron and calcium, dioxide-containing silica 40-60% wherein, alumina content 17-35%, iron oxide content 2-15%, calcium oxide content 1-10% extracts these useful matteies from flyash, becomes the focus of flyash higher value application.And current flyash higher value application mainly concentrates on the extraction aspect of aluminum oxide.
Treated coal ash is broadly divided into alkaline process and acid system both at home and abroad.In the sixties in last century, Poland just utilizes soda-lime sintering process to extract aluminum oxide from flyash, has built up the pilot plant that produces 5000 tons of aluminum oxide and 350,000 tons of cement per year.China Anhui Province Institute of Metallurgical Technology and Anhui Cement research institute combine and have declared by limestone sintering in the eighties, and aluminum oxide is extracted in the sodium carbonate stripping from flyash, and residue is for the production of the achievement of cement, and have passed through expert statement.Although alkaline process treated coal ash report is a lot, has no at present industrialized report.Its reason is that alkali process is tediously long, and facility investment is large, and energy consumption is high, cost is high, and the level of residue produced is the several times of flyash, a large amount of cement market goods locally difficulties that residue is made, comprehensive benefit is poor, thereby has hindered the application of alkaline process aspect total utilization of PCA.
With alkaline process, compare, acidic process flyash has obvious advantage.Acid system, when effectively extracting aluminum oxide, can obtain the silicon product, can be made into white carbon black after further processing and sells.The acid technological process facility investment is little, and energy consumption is low, and cost is also low, and level of residue is little, but the conversion unit manufacture of using has certain difficulty.Moreover flyash is the fine particles formed after high-temp combustion, wherein glassy phase and corundum have accounted for more than 80%, have had a strong impact on the activity of flyash and acid-respons.Therefore, need to improve flyash and sour reactive behavior to improve the solubility rate of aluminum oxide etc.Bibliographical information more be the acidleach negate should in the interpolation solubility promoter (as NH
4what CaF of F), but solubility rate is still lower, only has 35-45%, and resource utilization is low, and has added the fluorine element that environment is had to pollution, has caused secondary pollution.In a word, the higher value application of current flyash is only focused on the wherein extraction of one or two kind of element (being mainly aluminium), and has ignored wherein silicon, iron, and the extraction of the elements such as calcium, be difficult to produce economic benefit.
Summary of the invention
The purpose of this invention is to provide a kind of step-by-step precipitation method that extracts aluminium, silicon, iron and calcium constituent from flyash, to realize the comprehensive higher value application of flyash, low to overcome the resource utilization that prior art exists, environment is caused to secondary pollution, or ignored the wherein deficiencies such as extraction of the elements such as silicon, iron, calcium.
The present invention takes following technical scheme: it comprises the following steps:
(1) flyash is ground to the 200-400 order, at 800-1000 ℃ of lower calcination activation 1-3 hour; By the flyash after roasting and mixed in hydrochloric acid, be heated to 90-150 ℃ of reaction 1-3 hour, and obtain filter residue and filtrate after filtering; Filter residue is further processed and is obtained white carbon black;
(2) the filtrate pH value that set-up procedure (1) obtains is 1.5-3.5, after precipitation, filtration, obtains filter residue and filtrate, and filter residue, through washing, obtains the compound of iron after oven dry;
(3) the filtrate pH value that set-up procedure (2) obtains is 3.8-5.2, after precipitation, filtration, obtains filter residue and filtrate, and filter residue obtains aluminium hydroxide after washing, oven dry, further after calcining, obtains metallurgical-grade aluminum oxide;
(4) filtrate step (3) obtained obtains Calcium dichloride dihydrate after about 100 ℃ evaporations, further after calcination, obtains Calcium Chloride Powder Anhydrous.
Preferably, the concentration of hydrochloric acid in described step (1) is 34-36%.
Preferably, the industry of the flyash adapted 1.8-2 ton after the activation per ton in described step (1) concentrated hydrochloric acid.
Preferably, the filter residue in described step (2) obtains iron oxide yellow about 100 ℃ oven dry, and iron oxide yellow can obtain red iron oxide 240-260 ℃ of calcination.
Preferably, the aluminium hydroxide obtained in described step (3) can obtain metallurgical-grade aluminum oxide in 40-100 minute 1050 ℃ of calcinings.
Preferably, the Calcium dichloride dihydrate obtained in described step (4) obtains Calcium Chloride Powder Anhydrous 250-280 ℃ of calcination.
Four above-mentioned steps form the comprehensive higher value application technique of complete flyash; Simultaneously, wherein any one step in four steps is added together with the content be associated in other step, also forms four and is mutually related again independently of one another, and be the complete comprehensive higher value application technique of flyash.
According to technique of the present invention, white carbon black can be extracted from flyash, iron oxide yellow, red iron oxide, aluminum oxide, Calcium dichloride dihydrate, the many kinds of substances such as Calcium Chloride Powder Anhydrous.Through chemical examination, every product purity is high, and all technical all meets national relevant technologies specification of quality.(suppose silicon oxide-containing 50% in flyash by 200,000,000 tons of China's flyash annual emissions, aluminum oxide 30%, ferric oxide 2%, calcium oxide 4%), the rate of recovery gets 70%, can produce 0.4 hundred million tons of metallurgical-grade aluminum oxides, 0.03 hundred million ton of red iron oxide, 0.7 hundred million tons of white carbon blacks, 0.1 hundred million tons of Calcium dichloride dihydrates, annual value of production is up to 4,638 hundred million yuan, and economic benefit is very considerable.And of the present invention simple for process, reasonable in design, required equipment is also fairly simple, invests little.The comprehensive higher value application technique of flyash of the present invention has overcome the problem of environmental pollution of flyash effectively, has greatly reduced the harm of flyash.
The various products that extract from flyash have been widely used.As red iron oxide can be used as rubber, paint, the tinting material of plastics etc.Iron oxide yellow can be used as pigment, the catalyzer of rust-inhibiting paint and organic synthesis, waste water conditioner etc.Aluminum oxide can be used as the basic raw material of electrolytic aluminum, and then can produce various aluminiums etc.Calcium Chloride Powder Anhydrous can be used as refrigeration agent, the condensation agent, and tackiness agent, and Calcium dichloride dihydrate can be made frostproofer, refrigeration agents etc., having extensive use aspect medicine and nonferrous smelting.White carbon black can be used as the strengthening agent of rubber plastic etc.
The present invention is the difference of utilizing precipitation character in the solution different at pH value of different from the acid-respons ability and different compounds of each compound in flyash, the metallic compound that will extract is separated from the flyash of complicated component, and purified, this is theoretical foundation of the present invention and basic skills.
With the method for other treated coal ash, compare, advantage of the present invention has:
(1) the present invention adopts the calcination for activation technology, at normal pressure, does not use any solubility promoter, with hydrochloric acid, just can make the aluminum oxide in flyash, ferric oxide, and the useful matteies such as calcium oxide effectively leach, and leaching yield is all more than 80%.
(2) the present invention adopts simple chemical precipitation method, by the silicon in flyash, and aluminium, iron, the useful elements such as calcium extract, and economic benefit is high, has realized the comprehensive higher value application of flyash.
(3) technique of the present invention can be extracted white carbon black from flyash, iron oxide yellow, and red iron oxide, aluminum oxide, Calcium dichloride dihydrate, the multiple products such as Calcium Chloride Powder Anhydrous, various products have been widely used, and added value of product is high.
(4) technological process of the present invention is simple, invests littlely, and cost is low, and added value of product is high, is a flyash that has the prospect comprehensive utilization industrialization method that becomes more meticulous.
The accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Embodiment 1
(1) somewhere flyash (chemical constitution is in Table 1) is ground to the 200-400 order, 800 ℃ of lower calcination activations 2 hours.Get 1 kilogram, flyash after roasting and 1.8 kilogram-mass marks and be about 35% concentrated hydrochloric acid and mix, 90 ℃ of reactions 1.5 hours, and obtain filter residue and filtrate after filtering.Filter residue obtains white carbon black after washing further processing, and the extraction yield of knowing as calculated silicon is 95%.
(2) the filtrate pH value that set-up procedure (1) obtains is 3.2, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains iron oxide yellow after drying under 100 ℃, iron oxide yellow obtains red iron oxide 260 ℃ of calcinations, and the extraction yield of knowing as calculated iron is 73%.
(3) the filtrate pH value that set-up procedure (2) obtains is 5.1, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains aluminium hydroxide after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 ℃ of calcinings after 50 minutes, and the extraction yield of knowing as calculated aluminium is 75%
(4) filtrate step (3) obtained, about 100 ℃ evaporations, during evaporation, when calcium chloride content reaches 60-70%, can be injected pail pack, obtains Calcium dichloride dihydrate after condensation.Calcium dichloride dihydrate can make Calcium Chloride Powder Anhydrous 260 ℃ of lower calcinations, and the extraction yield of knowing as calculated calcium is 77%.
Table 1 flyash chemical constitution
| Form | Al 2O 3 | SiO 2 | Fe 2O 3 | CaO | TiO 2 | K 2O | Na 2O | MgO | Alkali burns | Other | Amount to |
| % | 48.20 | 38.33 | 1.85 | 3.42 | 1.1 | 0.33 | 0.21 | 0.09 | 5.21 | 1.26 | 100.00 |
Embodiment 2
(1) by chemical constitution, somewhere flyash as shown in table 1 was ground to the 200-400 order, 800 ℃ of lower calcination activations 1 hour.Get 1 kilogram, flyash after roasting and 1.5 kilogram-mass marks and be about 34% concentrated hydrochloric acid and mix, 100 ℃ of reactions 1 hour, and obtain filter residue and filtrate after filtering.Filter residue obtains white carbon black after washing further processing, and the extraction yield of knowing as calculated silicon is 96%.
(2) the filtrate pH value that set-up procedure (1) obtains is 2.2, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains iron oxide yellow after drying under 100 ℃, iron oxide yellow obtains red iron oxide 260 ℃ of calcinations, and the extraction yield of knowing as calculated iron is 53%.
(3) the filtrate pH value that set-up procedure (2) obtains is 4.4, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains aluminium hydroxide after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 ℃ of calcinings after 50 minutes, and the extraction yield of knowing as calculated aluminium is 58.%
(4) filtrate step (3) obtained, about 100 ℃ evaporations, during evaporation, when calcium chloride content reaches 60-70%, can be injected pail pack, obtains Calcium dichloride dihydrate after condensation.Calcium dichloride dihydrate can make Calcium Chloride Powder Anhydrous 260 ℃ of lower calcinations, and the extraction yield of knowing as calculated calcium is 62%.
Embodiment 3
(1) by chemical constitution, somewhere flyash as shown in table 1 was ground to the 200-400 order, 900 ℃ of lower calcination activations 3 hours.Get 1 kilogram, flyash after roasting and 2 kilogram-mass marks and be about 36% concentrated hydrochloric acid and mix, 150 ℃ of reactions 3 hours, and obtain filter residue and filtrate after filtering.Filter residue obtains white carbon black after washing further processing, and the extraction yield of knowing as calculated silicon is 97%.
(2) the filtrate pH value that set-up procedure (1) obtains is 3.5, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains iron oxide yellow after drying under 100 ℃, iron oxide yellow obtains red iron oxide 260 ℃ of calcinations, and the extraction yield of knowing as calculated iron is 78%.
(3) the filtrate pH value that set-up procedure (2) obtains is 5.1, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains aluminium hydroxide after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 ℃ of calcinings after 50 minutes, and the extraction yield of knowing as calculated aluminium is 79%
(4) filtrate step (3) obtained, about 100 ℃ evaporations, during evaporation, when calcium chloride content reaches 60-70%, can be injected pail pack, obtains Calcium dichloride dihydrate after condensation.Calcium dichloride dihydrate can make Calcium Chloride Powder Anhydrous 260 ℃ of lower calcinations, and the extraction yield of knowing as calculated calcium is 76%.
Embodiment 4
(1) by chemical constitution, somewhere flyash as shown in table 1 was ground to the 200-400 order, 1000 ℃ of lower calcination activations 2 hours.Get 1 kilogram, flyash after roasting and 1.6 kilogram-mass marks and be about 34% concentrated hydrochloric acid and mix, 120 ℃ of reactions 2 hours, and obtain filter residue and filtrate after filtering.Filter residue obtains white carbon black after washing further processing, and the extraction yield of knowing as calculated silicon is 96%.
(2) the filtrate pH value that set-up procedure (1) obtains is 3.0, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains iron oxide yellow after drying under 100 ℃, iron oxide yellow obtains red iron oxide 260 ℃ of calcinations, and the extraction yield of knowing as calculated iron is 75%.
(3) the filtrate pH value that set-up procedure (2) obtains is 4.8, obtain filter residue and filtrate after precipitation, filtration, filter residue, through washing, obtains aluminium hydroxide after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 ℃ of calcinings after 50 minutes, and the extraction yield of knowing as calculated aluminium is 72%
(4) filtrate step (3) obtained, about 100 ℃ evaporations, during evaporation, when calcium chloride content reaches 60-70%, can be injected pail pack, obtains Calcium dichloride dihydrate after condensation.Calcium dichloride dihydrate can make Calcium Chloride Powder Anhydrous 260 ℃ of lower calcinations, and the extraction yield of knowing as calculated calcium is 71%.
Claims (6)
1. a step-by-step precipitation method that extracts aluminium, silicon, iron and calcium constituent from flyash comprises the following steps:
(1) flyash is ground to the 200-400 order, at 800-1000 ℃ of lower calcination activation 1-3 hour; By the flyash after roasting and mixed in hydrochloric acid, be heated to 90-150 ℃ of reaction 1-3 hour, and obtain filter residue and filtrate after filtering, filter residue is further processed and is obtained white carbon black;
(2) the filtrate pH value that set-up procedure (1) obtains is 1.5-3.5, after precipitation, filtration, obtains filter residue and filtrate, and filter residue obtains the compound of iron after washing, oven dry;
(3) the filtrate pH value that set-up procedure (2) obtains is 3.8-5.2, after precipitation, filtration, obtains filter residue and filtrate, and filter residue obtains aluminium hydroxide after washing, oven dry, further after calcining, obtains metallurgical-grade aluminum oxide;
(4) filtrate step (3) obtained obtains Calcium dichloride dihydrate after about 100 ℃ evaporations, further after calcination, obtains Calcium Chloride Powder Anhydrous.
2. the step-by-step precipitation method that extracts aluminium, silicon, iron and calcium constituent from flyash according to claim 1, is characterized in that: the concentrated hydrochloric acid that the hydrochloric acid in step (1) is 30%-36%.
3. the step-by-step precipitation method that extracts aluminium, silicon, iron and calcium constituent from flyash according to claim 1 and 2 is characterized in that: the hydrochloric acid adapted ratio in step (1) is the flyash adapted 1.8-2 ton industry concentrated hydrochloric acid after activation per ton.
4. the step-by-step precipitation method that extracts aluminium, silicon, iron and calcium constituent from flyash according to claim 3, it is characterized in that: the filter residue in step (2) can obtain iron oxide yellow about 100 ℃ oven dry, and iron oxide yellow obtains red iron oxide 200-300 ℃ of calcination.
5. the step-by-step precipitation method that extracts aluminium, silicon, iron and calcium constituent from flyash according to claim 4 is characterized in that: the aluminium hydroxide obtained in step (3) obtains metallurgical-grade aluminum oxide in 20-120 minute 900-1100 ℃ of calcining.
6. the step-by-step precipitation method that extracts aluminium, silicon, iron and calcium constituent from flyash according to claim 5, it is characterized in that: the Calcium dichloride dihydrate obtained in step (4) obtains Calcium Chloride Powder Anhydrous 240-280 ℃ of calcination.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876253A (en) * | 2015-05-15 | 2015-09-02 | 南阳东方应用化工研究所 | Method for treating calcium in high-calcium fly ash |
| CN111252774A (en) * | 2020-01-19 | 2020-06-09 | 刘文治 | Method for producing silica sol by using desulfurized gypsum and fly ash through treating waste with waste |
| CN113753929A (en) * | 2021-08-26 | 2021-12-07 | 王俊 | Method for preparing high-whiteness aluminum hydroxide and silicon fertilizer from high-alumina fly ash |
| CN117446814A (en) * | 2023-12-21 | 2024-01-26 | 内蒙古科技大学 | Method for preparing calcium silicate by using gas slag |
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| US4130627A (en) * | 1977-06-20 | 1978-12-19 | Russ James J | Process for recovering mineral values from fly ash |
| GB2205558A (en) * | 1987-05-18 | 1988-12-14 | Lonhro Plc | Recovery of alumina from aluminosilicates |
| CN101200305A (en) * | 2007-07-26 | 2008-06-18 | 李文志 | Coal ash roller type fine extractive technique |
| CN102241410A (en) * | 2010-05-14 | 2011-11-16 | 东北大学 | Ecological synthetic utilization method of fly ash |
| CN102344171A (en) * | 2010-07-30 | 2012-02-08 | 孙建之 | New method for resource comprehensive utilization of red mud and fly ash |
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2012
- 2012-06-12 CN CN201210191291.8A patent/CN103482707A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4130627A (en) * | 1977-06-20 | 1978-12-19 | Russ James J | Process for recovering mineral values from fly ash |
| GB2205558A (en) * | 1987-05-18 | 1988-12-14 | Lonhro Plc | Recovery of alumina from aluminosilicates |
| CN101200305A (en) * | 2007-07-26 | 2008-06-18 | 李文志 | Coal ash roller type fine extractive technique |
| CN102241410A (en) * | 2010-05-14 | 2011-11-16 | 东北大学 | Ecological synthetic utilization method of fly ash |
| CN102344171A (en) * | 2010-07-30 | 2012-02-08 | 孙建之 | New method for resource comprehensive utilization of red mud and fly ash |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876253A (en) * | 2015-05-15 | 2015-09-02 | 南阳东方应用化工研究所 | Method for treating calcium in high-calcium fly ash |
| CN111252774A (en) * | 2020-01-19 | 2020-06-09 | 刘文治 | Method for producing silica sol by using desulfurized gypsum and fly ash through treating waste with waste |
| CN113753929A (en) * | 2021-08-26 | 2021-12-07 | 王俊 | Method for preparing high-whiteness aluminum hydroxide and silicon fertilizer from high-alumina fly ash |
| CN117446814A (en) * | 2023-12-21 | 2024-01-26 | 内蒙古科技大学 | Method for preparing calcium silicate by using gas slag |
| CN117446814B (en) * | 2023-12-21 | 2024-03-26 | 内蒙古科技大学 | Method for preparing calcium silicate by using gas slag |
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Application publication date: 20140101 |