CN104772214B - A kind of method that fly ash highly removes ferrum - Google Patents
A kind of method that fly ash highly removes ferrum Download PDFInfo
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- CN104772214B CN104772214B CN201510174024.3A CN201510174024A CN104772214B CN 104772214 B CN104772214 B CN 104772214B CN 201510174024 A CN201510174024 A CN 201510174024A CN 104772214 B CN104772214 B CN 104772214B
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Abstract
The present invention provides a kind of method that fly ash highly removes ferrum, the fine powder of raw material flyash is sequentially passed through reduction, magnetic separation, hydrochloric acid leaching process, finally gives Fe2O3Content is less than 0.02% flyash.Beneficial effects of the present invention are：Technological operation is simple, and de-ironing efficiency is high, can make the Fe in flyash2O3Content is down to less than 0.02%, and calcium impurities also can remove in the lump, and removes the molecular sieve quality height that the flyash after ferrum is prepared, its Fe using the method2O3Content is less than commercially available value, iron ion both can have been avoided to block the duct of molecular sieve, can improve the cycle life of adsorption/desorption again.Additionally, this method can also reclaim in magnetic separation process obtains iron powder, for making steel.
Description
Technical field
The present invention relates to a kind of method that flyash reduces high-efficient deferrization.
Background technology
Flyash be coal or coal dust firing after fine particle shape residue, be the larger industrial residue of the current discharge capacity of China
One of.Nineteen ninety-five China's flyash discharge capacity reaches 1.25 hundred million tons, is about 1.5 hundred million tons within 2000, reaches 300,000,000 tons, according to special within 2010
Family's prediction China's flyash discharge capacity in 2015 is up to 5.7 hundred million tons, and substantial amounts of flyash is untreated to produce airborne dust, pollution
Air, can cause river to silt up if entering water system, and toxic and harmful substance therein also can cause to human body and biology to endanger
Evil.The comprehensive utilization of flyash is turned waste into wealth, it has also become an important techno-economic policy in China's economic construction, is to solve
The important means of contradiction between China's power generation environmental pollution and resource shortage.At present flyash is mainly as construction material,
For warming plate, slag cements, wall brick, floor etc., its usage amount is big, and utilization rate reaches 67%, but added value of product is not high.Powder
The main component of coal ash is silicon oxide and aluminium oxide, and wherein silica content accounts for more than 70%, and silicon oxide and aluminium oxide are also point
The main component of son sieve, molecular sieve is expensive, is to improve it to utilize added value with cheap coal ash for manufacturing for molecular sieve
Important channel.The application of molecular sieve widely, can be used for dehydration, drying, separation and the purification of gas or liquid, also may be used
It is used for all kinds of reactions as adsorbent, catalyst and ion-exchanger, in petrochemical industry, fine chemistry industry, agricultural, environmental conservation
Play an important role in field.Both raw material can have been saved using coal ash for manufacturing for molecular sieve, with simple flow and can set again
Standby, it is that large-scale production and the extensive application of molecular sieve creates conditions.
With the research of flyash synthesis of molecular sieve from 1985 by Holler and Wrisching, due to ring in recent years
Border protection work causes global extensive concern, and the research to flyash synthesis of molecular sieve is increasingly burning hot both at home and abroad, thus opens
The molecular sieve species sending also gets more and more, but flyash is not pure aluminosilicate after all, in addition to containing valuable element sial
Also contain significant component of ferrum element so that the molecular sieve preparing is mutually impure, not only easily block the duct of molecular sieve,
And make the exchange capacity of molecular sieve and cycle performance low.Therefore, need to flyash before with coal ash for manufacturing for molecular sieve
Carry out pretreatment, remove ferrum therein.
Document with regard to deferrization of pulverized coal ash is more, and mainly magnetic separation and pickling removes ferrum.Invention CN10272561B and
CN201848307U adopts magnetic separation mode to remove ferrum, but because the ferrum in flyash is mainly ferric iron, and trivalent ferromagnetism is faint,
Therefore effect is poor；Patent CN103131860A adopts after adding alkali calcining and activating flyash plus nitration mixture leaching removes ferrum, this mode
Big to the consumption of soda acid it is impossible to remove the whole ferrum in flyash；Northeast Petroleum University's Master's thesis of 2014 with
Powdered coal ash can not remove fine coal by the way of the research that two-step method prepares ZSM-5 molecular sieve also reports and only relies on acidleach
Whole ferrum in ash；Patent CN103833061A adopts combination method to remove ferrum flyash dissolution fluid, and the method can be by solution
Iron ion remove, but the ferrum in solid phase is produced little effect.
Content of the invention
The various problems existing for prior art, the present invention provides a kind of method that fly ash highly removes ferrum.The present invention
Technical scheme be：
A kind of method that fly ash highly removes ferrum, comprises the following steps that：
（1）By the fine powder of raw material flyash and reducing agent in nitrogen protection or with nitrogen under conditions of to carry out reduction anti-
Should, reaction temperature is 800～1100 DEG C, response time 20～60min, and the consumption of reducing agent is flyash according to stoichiometric proportion
1.5～2 times of middle ferrum element amount；
（2）3 magnetic separation are carried out to the flyash of reduction, magnetic field intensity is 465-744kA m-1；
（3）Flyash after magnetic separation is stirred 4h with 10% hydrochloric acid solution under conditions of temperature is 60 °C leached,
The flyash except ferrum is obtained after filtration drying.
Fe in the fine powder of described raw material flyash2O3Content be 4.42-7.84%, Task-size Controlling is in below 0.042mm.
The reducing agent of described reduction reaction is coal dust, coke blacking, carbon monoxide, coal gas or hydrogen.
Described its Fe of the flyash except ferrum2O3Content is less than 0.02%.
Beneficial effects of the present invention：The method that a kind of fly ash highly that the present invention provides removes ferrum, technological operation is simple, removes
Ferrum efficiency high, can make the Fe in flyash2O3Content is down to less than 0.02%, and calcium impurities also can remove in the lump, and utilizes the party
The molecular sieve quality that method is prepared except the flyash after ferrum is high, its Fe2O3Content is less than commercially available value, and iron ion both can have been avoided to block
The duct of molecular sieve, can improve the cycle life of adsorption-desorption again.Additionally, this method can also reclaim in magnetic separation process obtaining
Iron powder, falls for steel-making.
Brief description
Fig. 1 is the standby molecular screen primary powder color contrast figure of coal ash for manufacturing that different method for removing iron obtain；
Fig. 2 is the process chart of the inventive method.
Specific embodiment
The flyash that the present invention implements to adopt derives from Shanxi Huaneng Group steam power plant.
The present invention implements the reducing agent adopting（Coal dust, coke blacking, coal gas or hydrogen）, hydrochloric acid be commercially available prod.
The present invention implements to carry out magnetic separation using CXG Φ 50 type magnetic separator.
Embodiment 1
It is reducing agent using anchracite duff, processing step is as follows：
（1）The fine powder of raw material flyash and anchracite duff are carried out reduction reaction, reaction temperature under conditions of with nitrogen
Spend for 1000 DEG C, response time 40min, the consumption of reducing agent is according to 1.5 times of stoichiometric proportion；
（2）3 magnetic separation are carried out to the flyash of reduction, magnetic field intensity is 465kA m-1；
（3）By the flyash after magnetic separation with 10% hydrochloric acid solution under conditions of 60 °C of temperature stirring 4h leached, mistake
Be filtered dry dry after obtain Fe2O3Content is 0.019% iron power removing coal ash.
Embodiment 2
It is reducing agent using coke, processing step is as follows：
（1）The fine powder of raw material flyash and coke are carried out reduction reaction under conditions of with nitrogen, reaction temperature is
900 DEG C, response time 50min, the consumption of reducing agent is according to 1.8 times of stoichiometric proportion；
（2）3 magnetic separation are carried out to the flyash of reduction, magnetic field intensity is 500kA m-1；
（3）By the flyash after magnetic separation with 10% hydrochloric acid solution under conditions of 60 °C of temperature stirring 4h leached, mistake
Be filtered dry dry after obtain Fe2O3Content is 0.015% iron power removing coal ash.
Embodiment 3
It is reducing agent using hydrogen, processing step is as follows：
（1）The fine powder of raw material flyash and hydrogen are carried out reduction reaction under nitrogen protection, reaction temperature is 1100 DEG C,
Response time 20min, the consumption of reducing agent is 2 times of the fine powder consumption of raw material flyash according to stoichiometric proportion；
（2）3 magnetic separation are carried out to the flyash of reduction, magnetic field intensity is 650 kA m-1；
（3）By the flyash after magnetic separation with 10% hydrochloric acid solution under conditions of 60 °C of temperature stirring 4h leached, mistake
Be filtered dry dry after obtain Fe2O3Content is 0.013% iron power removing coal ash.
Embodiment 4
It is reducing agent using coal gas, processing step is as follows：
（1）The fine powder of raw material flyash and coal gas are carried out reduction reaction under nitrogen protection, reaction temperature is 800 DEG C,
Response time 60min, the consumption of reducing agent is 1.9 times of the fine powder consumption of raw material flyash according to stoichiometric proportion；
（2）3 magnetic separation are carried out to the flyash of reduction, magnetic field intensity is 744 kA m-1；
（3）By the flyash after magnetic separation with 10% hydrochloric acid solution under conditions of 60 °C of temperature stirring 4h leached, mistake
Be filtered dry dry after obtain Fe2O3Content is 0.017% iron power removing coal ash.
Table 1 removes ferrum through the molecular sieve that the flyash that the inventive method removes ferrum is prepared with merely through magnetic separation-salt Ore Leaching
The molecular sieve performance that flyash is prepared compares
| System with molecular sieve for preparing is for approach | Outward appearance | Fe2O3Content | The cycle life (secondary) of adsorption-desorption |
| Prepared by the inventive method | White solid | <0.02% | 5000 |
| Magnetic separation-salt Ore Leaching preparation | Yellow solid | 1.82～2.76% | 200 |
Claims (2)
1. a kind of fly ash highly removes the method for ferrum it is characterised in that comprising the following steps that：
(1) by Fe2O3Content is 4.42-7.84%, the fine powder of the raw material flyash in below 0.042mm for the Task-size Controlling and reduction
Agent carries out reduction reaction under conditions of nitrogen protection, and reaction temperature is 800～1100 DEG C, response time 20～60min, reduction
The consumption of agent is 1.5～2 times of ferrum element amount in flyash according to stoichiometric proportion；
(2) 3 magnetic separation are carried out to the flyash of reduction, magnetic field intensity is 465-744kA m-1；
(3) flyash after magnetic separation is stirred 4h with 10% hydrochloric acid solution under conditions of temperature is 60 DEG C to be leached, mistake
Be filtered dry dry after obtain Fe2O3Content is less than 0.02% flyash.
2. a kind of fly ash highly according to claim 1 remove ferrum method it is characterised in that described reduction reaction also
Former dose is coal dust, coke blacking, carbon monoxide, coal gas or hydrogen.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105502464B (en) * | 2015-12-15 | 2017-09-26 | 合肥学院 | Ferro element separates except technique in a kind of titanium gypsum |
| CN111057810B (en) * | 2019-11-25 | 2021-10-08 | 中国石油化工股份有限公司 | Method for removing impurity iron in gasified slag |
| CN112725842A (en) * | 2020-12-28 | 2021-04-30 | 郑州大学 | Method for preparing aluminum-silicon-based alloy by using fly ash |
| CN113499855B (en) * | 2021-05-27 | 2024-05-17 | 中国地质科学院郑州矿产综合利用研究所 | Method for improving deironing effect of vitreous phase coal series waste by adopting microwave pretreatment |
| CN114212799B (en) * | 2021-12-21 | 2024-03-12 | 黑龙江省能源环境研究院 | Fly ash pretreatment method for molecular sieve preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| HUT56143A (en) * | 1985-12-11 | 1991-07-29 | Dunai Vasmu | Process for utilizing iron content of iron ores, iron oxide containing materials, by-products of iron and steel production and wastes |
| AU741669B2 (en) * | 1997-08-04 | 2001-12-06 | Bechtel Corporation | Method for direct reduction and upgrading of fine-grained refractory and earthy iron ores and slags |
| CN100446866C (en) * | 2003-12-26 | 2008-12-31 | 宝钢集团上海梅山有限公司 | Method for recovering iron concentrate from blast furnace dust |
| CN101869870A (en) * | 2010-04-27 | 2010-10-27 | 中国神华能源股份有限公司 | Method for magnetically separating and removing ion from fly ash |
| CN101811712A (en) * | 2010-04-27 | 2010-08-25 | 中国神华能源股份有限公司 | Method for preparing metallurgical-grade aluminum oxide by using fluid-bed fly ash |
| CN102241410B (en) * | 2010-05-14 | 2013-07-10 | 东北大学 | Ecological synthetic utilization method of fly ash |
| JP5772869B2 (en) * | 2013-04-24 | 2015-09-02 | 住友金属鉱山株式会社 | Method for producing hematite for iron making |
| CN103572040B (en) * | 2013-11-22 | 2015-02-04 | 中国矿业大学(北京) | Method for reducing carbon, sulfur and iron of fly ash and recovering iron ore concentrate |
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