CN113149718B - Method for preparing silicon-potassium compound fertilizer by using fly ash - Google Patents
Method for preparing silicon-potassium compound fertilizer by using fly ash Download PDFInfo
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- CN113149718B CN113149718B CN202110467950.5A CN202110467950A CN113149718B CN 113149718 B CN113149718 B CN 113149718B CN 202110467950 A CN202110467950 A CN 202110467950A CN 113149718 B CN113149718 B CN 113149718B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
- C01F7/0693—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process from waste-like raw materials, e.g. fly ash or Bayer calcination dust
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
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Abstract
A method for preparing a silicon-potassium compound fertilizer by using fly ash comprises the following steps: (1) mixing a potassium hydroxide solution with the fly ash to prepare a mixed slurry; (2) stirring and heating to 160-260 ℃ for leaching reaction; (3) solid-liquid separation is carried out on the leached materials to obtain transformation slag and transformation liquid; the solid component in the transformation slag is mainly KAlSiO 4 Washing with water and stoving to obtain the composite Si-K fertilizer. The method of the invention utilizes the mode of leaching the fly ash by potassium hydroxide solution, can be used as a silicon-potassium compound fertilizer, and realizes the harmless utilization of the fly ash; the potassium hydroxide solution is used for leaching the fly ash, so that part of alumina in the fly ash can be extracted.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of fly ash, and particularly relates to a method for preparing a silicon-potassium compound fertilizer by utilizing fly ash.
Technical Field
The fly ash is solid waste generated in the power generation process of a coal-fired power plant, a large amount of fly ash can be generated every year in the world, most of the fly ash is stored in a stockpiling mode, the comprehensive utilization rate is insufficient, and long-term stockpiling treatment not only occupies a large amount of land resources, but also pollutes the environment. The fly ash can be obtained by analyzing the component composition of the fly ash, contains some nutrient elements required by the growth of crops, has the advantages of good particle distribution and dispersibility, and can be considered to be made into a fertilizer for crop production, so that the utilization rate of the fly ash is improved.
In recent years, relevant practitioners have conducted a great deal of research work on the comprehensive utilization of fly ash, such as "a method for preparing a compound fertilizer using fly ash as a raw material, proposed by zheng jian citizen, publication no: the method of CN 102603407A ", the main steps include: (1) preparing raw materials according to the weight percentage of each component: urea, monoammonium phosphate, potassium sulfate, monopotassium phosphate, nano fly ash, humic acid, lignin, indoleacetic acid, water, chitosan, borax, zinc chloride, sodium molybdate, manganese sulfate, sodium dodecyl benzene sulfonate, ferrous sulfate, magnesium sulfate, copper sulfate and dimethyl sulfoxide; (2) mixing the raw materials in the step, putting the mixture into a reaction kettle, and stirring and reacting for 2 hours at the temperature of 100-120 ℃; (3) filtering the solution with a 200 mesh sieve to remove residues; (4) adding the nano fly ash into the filtering solution according to the weight percentage, and uniformly stirring to obtain the compound fertilizer.
The preparation method of the composite type controlled-release fertilizer taking fly ash as the raw material, which is proposed by Song dynasty Wu et al, discloses the following steps: the method of CN 102093129A "mainly comprises the following steps: (1) placing the fly ash in a crucible to be roasted in a muffle furnace, and carrying out acid dissolution treatment on the roasted fly ash by using 2mol/L acid to obtain pretreated fly ash; (2) mixing the pretreated fly ash, industrial aluminum hydroxide, sodium carbonate and polyaluminum chloride according to a ratio, and then placing the mixture in a muffle furnace for roasting for 1-3 hours to obtain a roasted product; (3) under the condition of stirring, completely immersing the roasted product into deionized water, heating to 30-80 ℃, and taking liquid to supplement alkali to be neutral; (4) heating to 100 ℃, and crystallizing under stirring; (5) and mixing and granulating the product obtained by filtering and drying and the nitrogen fertilizer according to a ratio to obtain the compound loss-control fertilizer.
Zhengweina proposes "a process for producing a compound fertilizer using sludge and fly ash, publication no: the method of CN 106064972A "mainly comprises the following steps: (1) adding straw powder and fly ash into the dewatered sludge and uniformly stirring; (2) carrying out microbial fermentation on the mixed material, and subjecting the material to middle-temperature, high-temperature and middle-temperature fermentation processes; (3) adding concentrated sulfuric acid into the fermented material, and stirring to react; (4) drying the reacted materials, adding a certain amount of monoammonium phosphate, monopotassium phosphate, potassium sulfate and magnesium sulfate, and uniformly mixing; (5) and (4) feeding the mixed material obtained in the step (4) into a granulator for granulation and forming, and then carrying out drying and activation treatment to obtain the compound fertilizer.
The existing method can also realize the comprehensive utilization of the fly ash, but has the problems of complex flow, long production period, more raw materials, increased production cost and the like. Therefore, it is urgently needed to invent a method which has simple process and higher practical value and can improve the utilization rate of the fly ash.
Disclosure of Invention
The invention aims to provide a method for preparing a silicon-potassium compound fertilizer by using fly ash, which overcomes the defects in the prior art, improves the comprehensive utilization rate of the fly ash, adopts a potassium hydroxide solution to leach the fly ash, can recover a potassium metaaluminate solution obtained after leaching, obtains an aluminum hydroxide product through carbonation decomposition, obtains an aluminum oxide product through roasting, and uses leaching slag as the silicon-potassium compound fertilizer for crop growth.
The method of the invention comprises the following steps:
1. mixing a potassium hydroxide solution and fly ash according to a liquid-solid ratio of 2-5 mL/g to prepare a mixed slurry; the concentration of the potassium hydroxide solution is 240-280 g/L;
2. heating the mixed slurry to 160-260 ℃ under the stirring condition to carry out leaching reaction for 30-90 min to obtain a leached material;
3. carrying out solid-liquid separation on the leached materials to obtain transformation slag and transformation liquid; the solid component in the transformation slag is mainly KAlSiO 4 Washing with water and stoving to obtain the composite Si-K fertilizer.
In the step 1, the fly ash contains Al according to mass percent 2 O 3 10～55％，CaO 0.5～10％，SiO 2 15～45％。
In the step 2, the main reaction formula of the leaching reaction is as follows:
3Al 2 O 3 ·2SiO 2 +6KOH→2KAl SiO 4 +4KAlO 2 +3H 2 O (1)。
in the step 3, the obtained transformation liquid is heated to 50-95 ℃, and then CO is introduced 2 Decomposition by carbonation of CO 2 Introducing for 1-7 h, and filtering and separating the obtained decomposed material to obtain a solid phase containing aluminum hydroxide; and drying the solid phase and roasting to prepare the alumina.
The reaction formula of the carbonation decomposition is as follows:
2KOH+CO 2 ＝K 2 CO 3 +H 2 o (2) and
2KAl(OH) 4 +CO 2 ＝K 2 CO 3 +2Al(OH) 3 +H 2 O (3)。
in the method, the yield of the aluminum oxide is 10-50%.
In the above method, the washing liquid is washed with water until the washing liquid is neutral, and the obtained washing liquid is mixed with the transformation liquid, followed by heating and carbonation decomposition.
In the method, after the fly ash is leached by potassium hydroxide solution, K in filter residue 2 Increased O content and Al content in fly ash 2 O 3 After being dissolved by alkali, part of the alkali enters a liquid phase, and the transformation liquid is subjected to carbonation decomposition and roasting to obtain an alumina product; part of Al 2 O 3 After being dissolved out, the rest Al 2 O 3 Remaining in the transformed slag to form potassium aluminosilicate.
Compared with the prior art, the invention has the characteristics and beneficial effects that: (1) the mode of leaching the fly ash by using the potassium hydroxide solution can be used as a silicon-potassium compound fertilizer, so that the harmless utilization of the fly ash is realized; (2) the potassium hydroxide solution is used for leaching the fly ash, so that part of alumina in the fly ash can be extracted.
Drawings
FIG. 1 is a flow chart of the method for preparing a silicon-potassium compound fertilizer by using fly ash.
Detailed Description
In the embodiment of the invention, the stirring speed of the leaching reaction is 200-400 rpm.
The fly ash adopted in the embodiment of the invention is the fly ash generated in the power generation process of a coal-fired power plant.
In the embodiment of the invention, the washing liquid is washed until the washing liquid is neutral, and the obtained washing liquid is mixed with the transformation liquid and then is heated and carbonated for decomposition.
In the case of carbonation decomposition in the examples of the present invention, CO 2 Is introduced in a total amount of CO 2 With K in transformation liquid + The molar ratio of (0.5-1.5): 1.
In the embodiment of the invention, the solid phase of the transformation slag contains 30-35% of silicon oxide and 21-27% of potassium oxide by mass.
In the embodiment of the invention, the liquid phase obtained by filtering and separating the decomposed material is a solution containing potassium carbonate, and the solution is causticized by adding alkali to prepare a potassium hydroxide solution which is used as a raw material for recycling.
Example 1
The flow is shown in figure 1:
mixing a potassium hydroxide solution and fly ash according to a liquid-solid ratio of 4mL/g to prepare a mixed slurry; the concentration of the potassium hydroxide solution is 240 g/L; the fly ash contains Al according to mass percent 2 O 3 47.72％，CaO 2.6％，SiO 2 38.76％，K 2 O 0.362％，Na 2 O 0.202％；
Heating the mixed slurry to 200 ℃ under the stirring condition for leaching reaction, wherein the leaching reaction time is 60min, and obtaining a leaching material;
carrying out solid-liquid separation on the leached materials to obtain transformation slag and transformation liquid; the solid component in the transformation slag is mainly KAlSiO 4 The silicon oxide content is 30.96 percent, the potassium oxide content is 21.80 percent, and the silicon-potassium compound fertilizer is prepared after washing and drying;
the obtained transformation liquid is heated to 65 ℃ and then CO is introduced 2 Carrying out carbonation decomposition for 6 hours, and filtering and separating the obtained decomposed material to obtain a solid phase containing aluminum hydroxide; drying the solid phase and roasting to prepare alumina; the yield of alumina was 20.3%.
Example 2
The method is the same as example 1, except that:
(1) mixing a potassium hydroxide solution and fly ash according to a liquid-solid ratio of 2mL/g to prepare a mixed slurry; the concentration of the potassium hydroxide solution is 260 g/L;
(2) carrying out leaching reaction at 160 ℃, wherein the leaching reaction time is 90 min; the solid content of the transformation slag is 33.77 percent of silicon oxide, and the content of the potassium oxide is 26.89 percent;
(3) the transformation liquid is heated to 55 ℃ and then CO is introduced 2 Carrying out carbonation decomposition for 7 hours, and filtering and separating the obtained decomposed material to obtain a solid phase containing aluminum hydroxide; drying the solid phase and roasting to prepare alumina; the yield of alumina was 31.43%.
Example 3
The method is the same as example 1, except that:
(1) mixing a potassium hydroxide solution and fly ash according to a liquid-solid ratio of 5mL/g to prepare a mixed slurry; the concentration of the potassium hydroxide solution is 280 g/L;
(2) leaching reaction is carried out at 260 ℃, and the leaching reaction time is 30 min; the solid content of the transformation slag is 34.13 percent of silicon oxide, and the content of the potassium oxide is 26.69 percent;
(3) the transformation liquid is heated to 95 ℃ and then CO is introduced 2 Performing carbonation decomposition, and introducing for 1h to obtain decomposed material, and filtering to separate solid phase containing aluminum hydroxide; drying the solid phase and roasting to prepare alumina; the yield of alumina was 29.78%.
Claims (4)
1. A method for preparing a silicon-potassium compound fertilizer by using fly ash is characterized by comprising the following steps:
(1) mixing a potassium hydroxide solution and fly ash according to a liquid-solid ratio of 2-5 mL/g to prepare a mixed slurry; the concentration of the potassium hydroxide solution is 240-280 g/L;
(2) heating the mixed slurry to 160-260 ℃ under the stirring condition for leaching reaction, wherein the leaching reaction time is 30-90 min, and obtaining a leaching material; the main reaction formula of the leaching reaction is as follows:
3Al 2 O 3 ·2SiO 2 +6KOH→2KAl SiO 4 +4 KAlO 2 + 3 H 2 O （1）；
(3) extracting with ethanol to obtain extractCarrying out solid-liquid separation on the material to obtain transformation slag and transformation liquid; the solid component in the transformation slag is mainly KAlSiO 4 Washing with water and drying to obtain the silicon-potassium compound fertilizer; the obtained transformation liquid is heated to 50-95 ℃ and then CO is introduced 2 Decomposition by carbonation of CO 2 Introducing for 1-7 h, and filtering and separating the obtained decomposed material to obtain a solid phase containing aluminum hydroxide; and drying the solid phase and roasting to prepare the alumina.
2. The method for preparing the silicon-potassium compound fertilizer by using the fly ash as claimed in claim 1, wherein in the step (1), the fly ash contains Al according to mass percent 2 O 3 10~55%，CaO 0.5~10%，SiO 2 15~45%。
3. The method for preparing the silicon-potassium compound fertilizer by using the fly ash as claimed in claim 1, wherein the yield of the aluminum oxide is 10-50%.
4. The method for preparing a silicon-potassium compound fertilizer by using fly ash as claimed in claim 1, wherein in the step (3), the washing liquid is washed until the washing liquid is neutral, and the obtained washing liquid is mixed with the transformation liquid, and then is heated and carbonated for decomposition.
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| CN202110467950.5A CN113149718B (en) | 2021-04-28 | 2021-04-28 | Method for preparing silicon-potassium compound fertilizer by using fly ash |
| PCT/CN2021/096797 WO2022227182A1 (en) | 2021-04-28 | 2021-05-28 | Method for preparing silicon-potassium compound fertilizer by using fly ash |
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| CN1138704C (en) * | 2000-06-09 | 2004-02-18 | 中国石油天然气股份有限公司兰州石化分公司 | Method for treatment of waste lye |
| CN101591197A (en) * | 2008-05-26 | 2009-12-02 | 同方环境股份有限公司 | A kind of method of utilizing pre-desiliconizing with high alumina fly ash to prepare calcium silicate fertilizer |
| CN103145162A (en) * | 2013-01-08 | 2013-06-12 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | Method for producing alumina by coal ash |
| CN103771471B (en) * | 2014-01-26 | 2015-02-25 | 乌鲁木齐金石徽龙矿业有限公司 | Method for preparing aluminum oxide through coal ash |
| CN105800653A (en) * | 2016-03-16 | 2016-07-27 | 酒泉钢铁(集团)有限责任公司 | Method for extracting aluminum oxide from fly ash on basis of soda-lime sintering process |
| CN108424207B (en) * | 2018-06-04 | 2021-03-16 | 国家能源投资集团有限责任公司 | Method for preparing silicon-potassium-containing compound fertilizer by using fly ash acid method aluminum extraction residues, silicon-potassium-containing compound fertilizer and fly ash utilization method |
| CN108976040B (en) * | 2018-09-12 | 2021-07-06 | 郑忆依 | Method for preparing slow release fertilizer by using fly ash |
| CN109231225A (en) * | 2018-10-09 | 2019-01-18 | 东北大学 | A method of comprehensive utilization flyash |
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