CN101054192B - Method of preparing crystal aluminum chloride from circulation fluid bed fly ash - Google Patents
Method of preparing crystal aluminum chloride from circulation fluid bed fly ash Download PDFInfo
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- CN101054192B CN101054192B CN200710055504A CN200710055504A CN101054192B CN 101054192 B CN101054192 B CN 101054192B CN 200710055504 A CN200710055504 A CN 200710055504A CN 200710055504 A CN200710055504 A CN 200710055504A CN 101054192 B CN101054192 B CN 101054192B
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Abstract
The present invention relates to a preparation method for crystalloid aluminum chlorate, in particular to a preparation method for crystalloid aluminum chlorate by using the circulating fluidized bedfly ash as raw material. By means of the better chemical activity of the aluminum contained in the circulating fluidized bed fly ash, the aluminum chlorate solution is obtained from the circulating fluidized bed fly ash by a direct acid dissolution process, and then the supernatant is obtained by separating the slag from the liquid in a setting tank, and the supernatant is concentrated and crystalled, finally, the solid crystalloid aluminum chlorate is obtained after spray drying. The present invention has a wide range of raw material, a low cost, a simple manufacturing process, quality product, less energy consumption, and meets the circular economy conception.
Description
Technical field:
The present invention relates to a kind of preparation method of crystal aluminum chloride, especially is the raw material production crystal aluminum chloride with the circulating fluid bed coal ash.
Background technology:
Combustion technology of circulating fluidized is a kind of novel coal technology, has coal-fired wide adaptability, low pollution emission, thermo-efficiency advantages of higher.The late nineteen eighties, this technology has obtained widespread use after introducing China, is that the newly-built coal gangue power plant of fuel has substantially all adopted this technology with coal gangue and low grade coal particularly, will progressively replace traditional coal-powder boiler combustion technology in this technology of coal fired power generation field.
Method at China's production crystal aluminum chloride mainly contains at present, aluminium ash single stage method, bauxite acid pasting etc.Aluminium ash single stage method is to be the method for raw material production polymerizable crystallizable aluminum chloride with aluminium processing leftover bits, contains objectionable impuritiess such as heavy metal in the aluminium ash raw material, and national relevant document has forbidden that the aluminium ash is used for drinking water treatment for the water purification agent product of raw material production; The bauxite acid pasting is to be raw material with aluminum-containing minerals such as bauxite, hard kaolines, the method for producing the crystal aluminum chloride water purification agent through means such as peracid are molten.But these class methods raw material sources are limited, along with the consumption day by day of resources such as bauxite, will seek a kind of new alternative materials and technology.
Circulating fluidized bed output flyash has many with traditional different physicochemical characteristic of coal furnace flyash, and particularly the Si that it contained, Al have very high chemically reactive.The circulating fluidized bed combustion temperature is about 850-900 ℃, and its lime-ash is based on chainotte matter mixing material, and main thing is calcined kaolinite mutually.Studies show that kaolinite calcining in 600-900 ℃ of temperature range can change active well amorphousness metakaolinite into, Si, the Al in the kaolinite has good active at this moment, and wherein the activity of Al reaches the highest about 900 ℃.The designed combustion temperature of Combustion technology of circulating fluidized is generally about 850-900 ℃, and this temperature range just in time is positioned at the active calcination temperature range of kaolinite optimum Al.This shows that the Al in the circulating fluid bed coal ash has good active, can consume less energy it is extracted, and make the crystal aluminum chloride product with simple relatively method through further processing.
Summary of the invention
Purpose of the present invention just is that providing a kind of at above-mentioned the deficiencies in the prior art is the method for raw material production crystal aluminum chloride with the circulating fluid bed coal ash.
The objective of the invention is to realize in the following manner;
Main raw material adopts circulating fluid bed coal ash, through the molten liquor alumini chloridi that makes of peracid, separates through slag liquid again, and condensing crystal obtains crystal aluminum chloride after the drying.
This method comprises following method steps:
A. sour molten: as the weighing of circulating fluidized bed ash to be placed acid-resistant reacting kettle, add a certain amount of hydrochloric acid, stirring, reacting by heating certain hour;
B. separate: carry out slag liquid after sour molten reaction finishes and separate, adopt subsider;
C. concentrate: the aluminum chloride clear liquid after slag liquid is separated is sent into and is carried out negative pressure in the concentration tank and concentrate;
D. crystallization: the mother liquor after concentrating is put into the buffering cooling tank, and cooling is separated out and obtained the crystal aluminum chloride crystal;
E. dry: that crystal aluminum chloride crystal drying is obtained product.
Purpose of the present invention can also realize in the following manner;
Described acid is hydrochloric acid; Concentration of hydrochloric acid is 10%～30%; The add-on ratio of hydrochloric acid and circulating fluid bed coal ash is 2～4 (ml/g); The temperature of the molten reaction of acid is 100 ℃; Drying is a spraying drying; The spraying drying temperature is 80 ℃～100 ℃.
Beneficial effect: the crystal aluminum chloride raw material of using the present invention's preparation is extensive, with low cost, and production technique is simple, and energy consumption is less, and good product quality meets circular economy concept.
Description of drawings:
Accompanying drawing: the process flow sheet of preparing crystal aluminum chloride from circulation fluid bed fly ash
Embodiment:
Raw material adopts North China heat power plant output circulating fluid bed coal ash, and its chemical ingredients is as shown in table 1.
Table 1 circulating fluid bed coal ash chemical ingredients (W
B%)
| Chemical ingredients | SiO 2 | Al 2O 3 | Fe 2O 3 | MgO | CaO | Na 2O | K 2O | LOI |
| Flyash | 44.16 | 49.80 | 1.16 | 0.35 | 0.43 | 0.42 | 0.38 | 2.9 |
Embodiment 1
Take by weighing circulating fluid bed coal ash 100 grams and place acid-resistant reacting kettle, add mass concentration and be 300 milliliters of 30% hydrochloric acid, 100 ℃ of continuous agitation conditions reacted 2 hours down, after hydrochloric acid stripping reaction finishes, soak the slag sedimentation through cooling, the general subsider that adopts, slag liquid is separated obtain supernatant liquor, aluminum chloride supernatant liquor after slag liquid separates is sent into and is carried out condensing crystal in the concentration tank, sediment is for soaking slag, through further washing, sedimentation, separate the back discharging, for improving settling property, can add the flocculation agent Polyacrylamide, the washing lotion of washing filter residue turns back in the acid-resistant reacting kettle to be utilized again; Concentration tank is an enamel pot, can lead to steam heating, in order to accelerate the speed of condensing crystal, can adopt negative pressure to concentrate, the mother liquor after concentrating is put into the buffering cooling tank, with decrease of temperature, crystalline aluminium begins to separate out, filter, filtrate enters liquid storage tank for reusing, and the crystal aluminum chloride that obtains is got the crystal aluminum chloride product through 90 ℃ of spraying dryings again.
Embodiment 2
Take by weighing circulating fluid bed coal ash 100 grams, add mass concentration and be 350 milliliters of 22.5% hydrochloric acid, 100 ℃ of continuous agitation conditions reacted 2 hours down, after hydrochloric acid stripping reaction finishes, soak the slag sedimentation through cooling, the general subsider that adopts, slag liquid is separated obtain supernatant liquor, aluminum chloride supernatant liquor after slag liquid separates is sent into and is carried out condensing crystal in the concentration tank, sediment is for soaking slag, through further washing, sedimentation, separate the back discharging, for improving settling property, can add the flocculation agent Polyacrylamide, the washing lotion of washing filter residue turns back in the acid-resistant reacting kettle to be utilized again; Concentration tank is an enamel pot, can lead to steam heating, in order to accelerate the speed of condensing crystal, can adopt negative pressure to concentrate, the mother liquor after concentrating is put into the buffering cooling tank, with decrease of temperature, crystalline aluminium begins to separate out, filter, filtrate enters liquid storage tank for reusing, and the crystal aluminum chloride that obtains is got the crystal aluminum chloride product through 100 ℃ of spraying dryings again.
Embodiment 3
Take by weighing circulating fluid bed coal ash 100 grams, add mass concentration and be 400 milliliters of 15% hydrochloric acid, 100 ℃ of continuous agitation conditions reacted 2 hours down, after hydrochloric acid stripping reaction finishes, soak the slag sedimentation through cooling, the general subsider that adopts, slag liquid is separated obtain supernatant liquor, aluminum chloride supernatant liquor after slag liquid separates is sent into and is carried out condensing crystal in the concentration tank, sediment is for soaking slag, through further washing, sedimentation, separate the back discharging, for improving settling property, can add the flocculation agent Polyacrylamide, the washing lotion of washing filter residue turns back in the acid-resistant reacting kettle to be utilized again; Concentration tank is an enamel pot, can lead to steam heating, in order to accelerate the speed of condensing crystal, can adopt negative pressure to concentrate, the mother liquor after concentrating is put into the buffering cooling tank, with decrease of temperature, crystalline aluminium begins to separate out, filter, filtrate enters liquid storage tank for reusing, and the crystal aluminum chloride that obtains is got the crystal aluminum chloride product through 80 ℃ of spraying dryings again.
Claims (5)
1. the method for a preparing crystal aluminum chloride from circulation fluid bed fly ash, it is characterized in that: main raw material adopts circulating fluid bed coal ash, through the molten liquor alumini chloridi that makes of persalt acid, the add-on ratio of hydrochloric acid and circulating fluid bed coal ash is 2～4ml/g, separate through slag liquid again, condensing crystal obtains crystal aluminum chloride after the drying;
This method comprises the steps:
A. sour molten: as circulating fluid bed coal ash to be placed acid-resistant reacting kettle, add a certain amount of hydrochloric acid, stirring, reacting by heating certain hour;
B. separate: carry out slag liquid after sour molten reaction finishes and separate, adopt subsider;
C. concentrate: the aluminum chloride clear liquid after slag liquid is separated is sent into and is carried out negative pressure in the concentration tank and concentrate;
D. crystallization: the mother liquor after concentrating is put into the buffering cooling tank, and cooling is separated out and obtained the crystal aluminum chloride crystal;
E. dry: that crystal aluminum chloride crystal drying is obtained product.
2. according to the method for claim 1, it is characterized in that: described concentration of hydrochloric acid is 10%～30%.
3. according to the method for claim 1, it is characterized in that: the temperature of sour molten reaction is 100 ℃.
4. according to the method for claim 1, it is characterized in that: the described drying of step e is a spraying drying.
5. according to the method for claim 1, it is characterized in that: the described drying temperature of step e is 80 ℃～100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710055504A CN101054192B (en) | 2007-04-10 | 2007-04-10 | Method of preparing crystal aluminum chloride from circulation fluid bed fly ash |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200710055504A CN101054192B (en) | 2007-04-10 | 2007-04-10 | Method of preparing crystal aluminum chloride from circulation fluid bed fly ash |
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| CN101054192A CN101054192A (en) | 2007-10-17 |
| CN101054192B true CN101054192B (en) | 2010-05-19 |
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| CN200710055504A Expired - Fee Related CN101054192B (en) | 2007-04-10 | 2007-04-10 | Method of preparing crystal aluminum chloride from circulation fluid bed fly ash |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811711A (en) * | 2010-04-27 | 2010-08-25 | 中国神华能源股份有限公司 | Method for extracting aluminum oxide from fly ash |
| CN102642857B (en) * | 2011-02-16 | 2015-06-17 | 贵阳铝镁设计研究院有限公司 | Process method for producing metal aluminium by high-alumina fly ash |
| CN103466774A (en) * | 2013-10-10 | 2013-12-25 | 兰州理工大学 | Method for producing compound coagulant by using fly ash |
| CN110902704A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing polyaluminum chloride by using fluidized bed fly ash |
| CN111233014B (en) * | 2020-03-04 | 2022-04-26 | 神华准能资源综合开发有限公司 | Method for enhanced dissolution of fly ash |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4331637A (en) * | 1981-04-20 | 1982-05-25 | Reynolds Metals Company | Process for purifying aluminum chloride |
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2007
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4331637A (en) * | 1981-04-20 | 1982-05-25 | Reynolds Metals Company | Process for purifying aluminum chloride |
Non-Patent Citations (4)
| Title |
|---|
| 王丽华.利用粉煤灰制备氯化铝溶液的实验研究.桂林工学院学报25 2.2005,25(2),202-204. |
| 王丽华.利用粉煤灰制备氯化铝溶液的实验研究.桂林工学院学报25 2.2005,25(2),202-204. * |
| 陆胜等.生态处理粉煤灰制备结晶氯化铝、聚合氯化铝的实验研究.粉煤灰 2.2003,(2),10-11. |
| 陆胜等.生态处理粉煤灰制备结晶氯化铝、聚合氯化铝的实验研究.粉煤灰 2.2003,(2),10-11. * |
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