CN113562993A - Method for preparing aluminate water treatment agent from fly ash by using sodium bicarbonate and carbide slag - Google Patents

Method for preparing aluminate water treatment agent from fly ash by using sodium bicarbonate and carbide slag Download PDF

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Publication number
CN113562993A
CN113562993A CN202110828352.6A CN202110828352A CN113562993A CN 113562993 A CN113562993 A CN 113562993A CN 202110828352 A CN202110828352 A CN 202110828352A CN 113562993 A CN113562993 A CN 113562993A
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China
Prior art keywords
fly ash
sodium bicarbonate
carbide slag
water treatment
treatment agent
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Pending
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CN202110828352.6A
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Chinese (zh)
Inventor
郑春明
任兆辉
郑海鑫
李敏婧
钟国强
赵迪
程香颖
刘瑞
季永力
雷正龙
杜昊天
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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Priority to CN202110828352.6A priority Critical patent/CN113562993A/en
Publication of CN113562993A publication Critical patent/CN113562993A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00Hydraulic cements
    • C04B7/32Aluminous cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00Hydraulic cements
    • C04B7/24Cements from oil shales, residues or waste other than slag
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00Hydraulic cements
    • C04B7/24Cements from oil shales, residues or waste other than slag
    • C04B7/26Cements from oil shales, residues or waste other than slag from raw materials containing flue dust, i.e. fly ash
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/10Production of cement, e.g. improving or optimising the production methods; Cement grinding

Abstract

The invention relates to a method for preparing an aluminate water treatment agent from fly ash by using sodium bicarbonate and carbide slag. Drying the fly ash, sodium bicarbonate and carbide slag in an oven; the mass fraction of the fly ash, the sodium bicarbonate and the carbide slag is 1: (0.4-1.2): (0.8-1.6) grinding and fully mixing; transferring the uniformly mixed and ground materials into a ceramic crucible, and roasting in a muffle furnace; setting the roasting temperature of a muffle furnace (700-; the obtained material is the aluminate water treatment agent. The removal efficiency of methylene blue is researched and can reach more than 90%. In the process of the invention, a large amount of alkali and acid are not needed, and the raw materials are two kinds of power plant waste residues. The purpose of making waste by waste is achieved, and the raw material cost is greatly saved; and the economic benefit is great, and the environment is not polluted.

Description

Method for preparing aluminate water treatment agent from fly ash by using sodium bicarbonate and carbide slag
Technical Field
The invention belongs to the field of water treatment, and particularly relates to a method for preparing an aluminate water treatment agent from fly ash by using sodium bicarbonate and carbide slag.
Background
The coal powder furnace coal ash is formed by quickly cooling coal after high-temperature combustion (1300-1400 ℃), and the main components of the coal powder furnace coal ash comprise aluminum oxide, ferric oxide, calcium oxide, aluminum oxide and the like. The alumina content in the high-alumina pulverized coal furnace fly ash can reach about 50 percent. The phase mainly comprises mullite, quartz, vitreous body and other inert substances, the particles are in a regular spherical shape, the structure is compact, the activity is poor, the particles are difficult to be directly extracted and utilized by an acid-soluble or alkali-soluble method, the inert substances in the fly ash need to be pretreated by a physical/chemical method and then alumina is extracted. However, the reserves of high-quality bauxite in China are small, and on the other hand, the high-quality bauxite is increasingly scarce in recent years due to the exploitation of the bauxite. The content of alumina in the fly ash is generally 17-35%, and the content of alumina in the fly ash in partial areas can be as high as 40-60%, so that the fly ash is an important non-traditional alumina resource.
In recent years, in order to solve the problems of precious and poor bauxite resources, environmental pollution caused by fly ash and the like in China, high-value utilization of fly ash becomes a research hotspot of various domestic colleges and schools and scientific research institutions.
Chinese patent N201710197423.0 discloses a process for extracting alumina from pulverized coal furnace fly ash by an acid method, which relates to a process for extracting alumina from pulverized coal furnace fly ash by an acid method, ammonium sulfate is added into the pulverized coal furnace fly ash for activation, then high-temperature calcination is carried out to obtain activated pulverized coal ash clinker, hydrochloric acid is added for heating and dissolution, and aluminum chloride dissolution liquid is obtained; and (3) introducing hydrogen chloride gas into the dissolution liquid for crystallization, carrying out solid-liquid separation and washing to obtain high-purity aluminum chloride hexahydrate crystals and waste acid liquid, and calcining the crystals to generate metallurgical-grade aluminum oxide. And adding inorganic salt chlorides such as calcium chloride or magnesium chloride into the waste acid, heating, extracting, distilling and recovering hydrochloric acid and hydrogen chloride gas, and reusing the hydrochloric acid and the hydrogen chloride gas in the dissolution and crystallization processes.
Chinese patent CN101041450B "clean production process for preparing alumina and white carbon black by using high alumina fly ash" takes sodium carbonate as ingredient, decomposes high alumina fly ash at medium temperature to generate acid-soluble aluminosilicate material, acid-soaks the sinter material with dilute sulphuric acid to separate alumina and silica in the high alumina fly ash; the obtained aluminum-containing liquid part is further processed to generate aluminum hydroxide precipitate, the aluminum hydroxide precipitate is calcined to prepare aluminum oxide, and the silica-containing colloidal part is purified, washed, dried and calcined to prepare inorganic silicon compound products such as white carbon black, silica aerogel, superfine silica, porous silica and the like.
Chinese patent CN101759210B, a method for extracting high-purity alumina and silica gel from fly ash, adopts the steps of cyclic activation, leaching, carbon separation, sodium carbonate and water recovery, silicon-aluminum separation, pyrolysis, hydrochloric acid recovery and the like to obtain the high-purity alumina and silica gel from the fly ash, and similarly Chinese patent CN101254933B, a method for extracting the high-purity alumina and silica gel from the fly ash, wherein the process can ensure that the extraction rate of the alumina and the silica gel in the fly ash reaches more than 90 percent.
The inventive methods in the above patents all suffer from the same problems: the consumption of acid and alkali is very large due to the limitation of chemical conditions, waste acid and waste alkali liquor are generated in the process and cannot be recycled, and the cost of raw materials is very high, so that the technologies are difficult to industrialize.
In conclusion, the method for extracting the aluminum salt from the fly ash by using the sodium bicarbonate and the carbide slag and preparing the aluminate water treatment agent can get rid of the problem that the traditional acid dissolution method for preparing the aluminate water treatment agent from the fly ash has low acid and alkali consumption, greatly saves the raw material cost, basically does not generate waste acid and waste lye in the process, and achieves the purpose of preparing waste by using waste.
Disclosure of Invention
Aiming at the technical defects that the technologies are difficult to industrialize due to the fact that acid and alkali are consumed in a large amount, cannot be recycled and high in raw material cost, the invention aims to solve the technical problems that: how to provide a method for preparing aluminate water treatment agent from fly ash industrially to the greatest extent by utilizing high added value of fly ash and saving acid and alkali consumption and reducing cost.
In order to solve the problems, the invention adopts the following technical scheme:
the method for preparing the aluminate water treatment agent from the fly ash by using the sodium bicarbonate and the carbide slag comprises the following steps:
(1) pretreatment of materials:
drying: drying the fly ash, sodium bicarbonate and carbide slag in an oven;
mixing and grinding: the mass fraction of the fly ash, the sodium bicarbonate and the carbide slag is 1: (0.4-1.2): (0.8-1.6) grinding and fully mixing;
(2) preparing aluminate water treatment agent:
roasting in a muffle furnace: transferring the uniformly mixed and ground material in the step (1) into a ceramic crucible, and roasting in a muffle furnace; setting the roasting temperature of a muffle furnace (700-; the obtained material is the aluminate water treatment agent.
Preferably, the drying conditions in the step (1) are as follows: the drying temperature of the oven is 60-100 ℃; the drying time is 1-5 h.
Preferably, the temperature rise rate in the muffle furnace in the step (2) is (5-10) DEG C/min.
A process for preparing aluminate water treating agent from powdered coal ash by use of sodium bicarbonate and calcium carbide dregs includes such steps as destroying and modifying the internal structure of powdered coal ash, extracting Al from powdered coal ash, and using Si element in powdered coal ash, and features that the sodium bicarbonate can destroy the mullite and quartz structure of powdered coal ash during high-temp calcining and the calcium carbide dregs can transform silicon dioxide into calcium silicate for producing cement. The method can get rid of the traditional acid dissolution method for preparing the aluminate water treatment agent from the fly ash. In the process of the invention, a large amount of alkali and acid are not needed, and the raw materials are two kinds of waste residues. The purpose of using waste to prepare waste is achieved, and the raw material cost is greatly saved.
The invention carries out the removal experiment on methylene blue: preparing (0.03-0.05) g/L methylene blue solution and (1-2) g/L Polyacrylamide (PAM) solution, and degrading the methylene blue by using the prepared aluminate water treatment agent; weighing (0.1-0.5) g of aluminate water treatment agent, adding into the prepared methylene blue solution, stirring for dissolving (0.5-1) h, and adding (1-3) mL of prepared PAM solution. After the precipitation is completed, the absorbance after and before degradation is measured by a spectrophotometer, and the removal rate is calculated.
Removal rate ═ (initial absorbance-absorbance after removal)/initial absorbance.
The invention can remove more than 90% of methylene blue.
In conclusion, the invention is optimized in that the aluminate water treatment agent is prepared from the fly ash, and the fly ash and the carbide slag which are used as raw materials are all waste residues of a power plant, so that the cost of the raw materials is greatly saved, and the aim of preparing waste by using waste is fulfilled. And the problem of pollution of solid waste of a thermal power plant is solved, products with high added values are extracted from the waste, and the economic benefit is greatly improved. Compared with the traditional alkaline method and acid method, the method does not produce red mud and desilication waste liquid, and contributes more to environmental protection.
In the invention, sodium bicarbonate and carbide slag are used for preparing the aluminate water treatment agent from the fly ash. The ratio of the materials has the greatest influence on the result.
In the invention, the roasting temperature is 700-1000 ℃, and the methylene blue removing efficiency is researched by changing the roasting temperature. The removal rate can reach more than 90 percent.
The method is characterized in that the heating roasting time is (1-5) h, and the roasting time is changed to research the removal efficiency of the methylene blue. The removal rate can reach more than 90 percent.
The method for preparing the aluminate water treatment agent from the fly ash greatly saves the raw material cost, has great economic benefit and does not pollute the environment.
Detailed Description
Example 1
Drying: respectively putting the fly ash, the sodium bicarbonate and the carbide slag into a clean beaker, putting the beaker into an oven, and setting the temperature and time of the oven; drying for 1h at 60 ℃. And drying the moisture in the materials, cooling to room temperature, and taking out to obtain the materials. Then 5g of fly ash and 8g of carbide slag are weighed, wherein the fly ash and the carbide slag are dried.
Mixing: 6g of the dried sodium bicarbonate in the step (1) is weighed, mixed with 5g of the fly ash and 8g of the carbide slag in the step (1), transferred to a mortar and fully ground. And then roasting the ground material at high temperature.
Thirdly, roasting: transferring the material to a ceramic crucible, covering the crucible with a cover, roasting in a muffle furnace, heating to 5 ℃/min at 700 ℃, roasting for 1h, naturally cooling to room temperature after roasting, and taking out a sample.
And step (iv) the material obtained after roasting is an aluminate water treatment agent which is used for removing methylene blue. The removal efficiency is 91 percent
Example 2
Drying: respectively putting the fly ash, the sodium bicarbonate and the carbide slag into a clean beaker, putting the beaker into an oven, and setting the temperature and time of the oven; drying for 2h at 80 ℃. And drying the moisture in the materials, cooling to room temperature, and taking out to obtain the materials. Then 5g of fly ash and 6g of carbide slag with dried moisture are weighed for later use.
Mixing: 3.5g of dried sodium bicarbonate in the step (i) is weighed, mixed with 5g of fly ash and 6g of carbide slag in the step (i), transferred into a mortar and fully ground. And then roasting the ground material at high temperature.
Thirdly, roasting: transferring the medium material to a ceramic crucible, covering the crucible with a cover, roasting in a muffle furnace, heating to 8 ℃/min, setting the temperature to 850 ℃, roasting for 3h, naturally cooling to room temperature after roasting, and taking out a sample.
And step (iv) the material obtained after roasting is an aluminate water treatment agent which is used for removing methylene blue. The removal efficiency is 92%.
Example 3
Drying: respectively putting the fly ash, the sodium bicarbonate and the carbide slag into a clean beaker, putting the beaker into an oven, and setting the temperature and time of the oven; drying for 5h at 100 ℃. And drying the moisture in the materials, cooling to room temperature, and taking out to obtain the materials. Then 5g of fly ash and 4g of carbide slag with dried moisture are weighed for later use.
Mixing: weighing 2g of dried sodium bicarbonate in the step I, mixing with 5g of fly ash and 4g of carbide slag in the step I, transferring into a mortar, and fully grinding. And then roasting the ground material at high temperature.
Thirdly, roasting: transferring the material to a ceramic crucible, covering the crucible with a cover, roasting in a muffle furnace, heating to 10 ℃/min at 1000 ℃, roasting for 5 hours, naturally cooling to room temperature after roasting, and taking out a sample.
And step (iv) the material obtained after roasting is an aluminate water treatment agent which is used for removing methylene blue. The removal efficiency is 95%.
While the methods and techniques of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and/or modifications of the methods and techniques described herein may be made without departing from the spirit and scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.

Claims (3)

1. The method for preparing the aluminate water treatment agent from the fly ash by using the sodium bicarbonate and the carbide slag is characterized by comprising the following steps of:
(1) pretreatment of materials:
drying: drying the fly ash, sodium bicarbonate and carbide slag in an oven;
mixing and grinding: the mass fraction of the fly ash, the sodium bicarbonate and the carbide slag is 1: (0.4-1.2): (0.8-1.6) grinding and fully mixing;
(2) preparing aluminate water treatment agent:
roasting in a muffle furnace: transferring the uniformly mixed and ground material in the step (1) into a ceramic crucible, and roasting in a muffle furnace; setting the roasting temperature of a muffle furnace (700-; the obtained material is the aluminate water treatment agent.
2. The method of claim 1, wherein the oven drying temperature (60-100) degrees centigrade; the drying time is 1-5 h.
3. The method of claim 1, wherein the muffle is heated at a rate of (5-10) C/min.
CN202110828352.6A 2021-07-22 2021-07-22 Method for preparing aluminate water treatment agent from fly ash by using sodium bicarbonate and carbide slag Pending CN113562993A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107570109A (en) * 2017-10-20 2018-01-12 新疆大学 A kind of method that carbide slag treated coal ash realizes its recycling
CN107930576A (en) * 2017-11-27 2018-04-20 吉林大学 A kind of preparation method of fly ash micro-sphere porous material and obtained porous material
CN111592001A (en) * 2020-05-31 2020-08-28 佛山经纬纳科环境科技有限公司 Method for preparing layered double hydroxide and white carbon black from fly ash

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107570109A (en) * 2017-10-20 2018-01-12 新疆大学 A kind of method that carbide slag treated coal ash realizes its recycling
CN107930576A (en) * 2017-11-27 2018-04-20 吉林大学 A kind of preparation method of fly ash micro-sphere porous material and obtained porous material
CN111592001A (en) * 2020-05-31 2020-08-28 佛山经纬纳科环境科技有限公司 Method for preparing layered double hydroxide and white carbon black from fly ash

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
郑峰伟: "《粉煤灰中铝铁浸出过程及动力学研究》", 《中国优秀硕士学位论文电子期刊 工程科技Ⅰ辑》 *

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