CN116216731A - Method for preparing aluminum silicon oxide by using fly ash and obtained aluminum silicon oxide - Google Patents
Method for preparing aluminum silicon oxide by using fly ash and obtained aluminum silicon oxide Download PDFInfo
- Publication number
- CN116216731A CN116216731A CN202310486528.3A CN202310486528A CN116216731A CN 116216731 A CN116216731 A CN 116216731A CN 202310486528 A CN202310486528 A CN 202310486528A CN 116216731 A CN116216731 A CN 116216731A
- Authority
- CN
- China
- Prior art keywords
- silicon oxide
- fly ash
- aluminum silicon
- alkali
- mass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a method for preparing aluminum silicon oxide by using fly ash and the obtained aluminum silicon oxide. The method comprises the following steps: (1) Mixing the fly ash with an alkali solution, performing alkali dissolution reaction, and filtering to obtain alkali-dissolved fly ash; (2) Providing an acid solution, and adding one or more of sodium fluoride, potassium fluoride and ammonium fluoride into the acid solution to obtain an acid leaching solution; (3) Adding the alkali-soluble fly ash obtained in the step (1) into the solution for acid leaching, performing acid leaching reaction, and filtering to obtain acid leached fly ash; and (4) roasting the acid leached fly ash to obtain the aluminum silicon oxide. The aluminum silicon oxide obtained by the method may have an iron element content of less than 0.40 mass% in terms of iron oxide and a calcium element content of less than 0.20 mass% in terms of calcium oxide.
Description
Technical Field
The present invention relates generally to the field of fly ash recycling technology, and more particularly, to a method for preparing aluminum silicon oxide by using fly ash and aluminum silicon oxide prepared by the method.
Background
The content of alumina in the coal after the coal is calcined can reach more than 50%, and the full utilization of the resources such as aluminum and silicon in the coal is an effective way for utilizing the coal ash with high added value. Accordingly, methods for preparing aluminum silicon oxide using fly ash are being developed and explored.
However, in the existing method for preparing aluminum silicon oxide by using fly ash, the content of impurities such as iron element, calcium element and the like in the prepared aluminum silicon oxide product is relatively high, the production time is long, and the large-scale production and application of the aluminum silicon oxide are limited.
Therefore, the following problems are to be solved: provided is a method for producing an aluminum-silicon oxide from fly ash, which can produce a high-quality aluminum-silicon oxide having a reduced content of impurities such as iron element and calcium element, and which can further shorten the production time.
Disclosure of Invention
The present invention has been made keeping in mind the above problems occurring in the prior art.
In a first aspect, the present invention relates to a process for preparing an aluminium silicon oxide comprising the steps of:
(1) Mixing fly ash with alkali solution, performing alkali dissolution reaction, and then subjecting the obtained reaction mixture to solid-liquid separation to obtain alkali-dissolved fly ash and alkali-dissolved liquid, and optionally subjecting the alkali-dissolved fly ash to washing and drying;
(2) Providing an acid solution, and adding fluoride to the acid solution to form an acid leaching solution, wherein the fluoride is selected from one or more of sodium fluoride, potassium fluoride and ammonium fluoride;
(3) Adding the alkali-soluble fly ash obtained in the step (1) into the acid leaching solution formed in the step (2), performing acid leaching reaction, and then subjecting the obtained reaction mixture to solid-liquid separation to obtain acid leached fly ash and acid leaching solution, and optionally subjecting the acid leached fly ash to washing and drying;
(4) Roasting the acid leached fly ash obtained in the step (3) to obtain aluminum silicon oxide.
In a second aspect, the present invention relates to an aluminium silicon oxide, obtainable by a process according to the first aspect.
The applicant found that when preparing aluminum silicon oxide from fly ash through alkali leaching treatment, acid leaching treatment and roasting treatment, by adding specific auxiliary agents (one or more of sodium fluoride, potassium fluoride and ammonium fluoride) into the acid leaching solution, the content of impurities such as iron element, calcium element and the like in the obtained aluminum silicon oxide can be effectively reduced, and meanwhile, the time of the acid leaching treatment can be greatly shortened, so that the production efficiency is further improved.
Drawings
These and/or other aspects will become apparent and more readily appreciated from the following description of the embodiments taken in conjunction with the accompanying drawings, wherein:
fig. 1 shows a schematic flow chart of an exemplary embodiment of a method for preparing aluminum silicon oxide using fly ash according to the present invention.
Detailed Description
In the field related to fly ash, since the form of each element in the fly ash existing in the system is complicated, for convenience of description, each element is generally referred to in terms of its oxide and its amount is expressed in terms of the amount of the oxide converted. This generic representation is also used herein. Thus, when reference is made herein to an oxide of an element, that oxide represents the various possible forms of the element in the system. Accordingly, when reference is made herein to the content of an oxide of an element, that content means the total content of the element in terms of its oxide.
In addition, it should also be understood that the expression "the content of the X element in terms of X oxide" herein means that the amount of the X element is converted in its oxide form as a constituent unit. For example, the expression "silicon element content in terms of silicon dioxide" means that the amount of silicon element is calculated as silicon dioxide (SiO 2 ) As constituent units, performing conversion; the expression "content of aluminum element in terms of alumina" means that the amount of aluminum element is expressed as aluminum oxide (Al 2 O 3 ) As constituent units, performing conversion; the expression "content of elemental iron in terms of iron oxide" means the amount of elemental iron in terms of iron oxide (Fe 2 O 3 ) As constituent units, performing conversion; the expression "calcium element content in terms of calcium oxide" means that the amount of calcium element is converted with calcium oxide (CaO) as a constituent unit. This is a common representation in the art, as will be readily appreciated by those skilled in the art.
In order to make the objects, technical solutions and advantageous technical effects of the present application clearer, the present application will be described in detail below. It should be noted that the various aspects, features, embodiments, and advantages thereof described herein may be compatible and/or may be combined together.
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The present invention relates to a method for preparing an aluminum silicon oxide and an aluminum silicon oxide prepared according to the method.
The present invention will be specifically described below.
Method for producing aluminum silicon oxide
In a first aspect, the present invention relates to a process for preparing an aluminium silicon oxide comprising the steps of:
(1) Mixing fly ash with alkali solution, performing alkali dissolution reaction, and then subjecting the obtained reaction mixture to solid-liquid separation to obtain alkali-dissolved fly ash and alkali-dissolved liquid, and optionally subjecting the alkali-dissolved fly ash to washing and drying;
(2) Providing an acid solution, and adding fluoride to the acid solution to form an acid leaching solution, wherein the fluoride is selected from one or more of sodium fluoride, potassium fluoride and ammonium fluoride;
(3) Adding the alkali-soluble fly ash obtained in the step (1) into the acid leaching solution formed in the step (2), performing acid leaching reaction, and then subjecting the obtained reaction mixture to solid-liquid separation to obtain acid leached fly ash and acid leaching solution, and optionally subjecting the acid leached fly ash to washing and drying;
(4) Roasting the acid leached fly ash obtained in the step (3) to obtain aluminum silicon oxide.
The steps will be described in detail below.
1. Step (1)
In step (1), the fly ash is mixed with an alkali solution, alkali dissolution reaction is carried out, then the obtained reaction mixture is subjected to solid-liquid separation to obtain alkali-dissolved fly ash and alkali-dissolved liquid, and the alkali-dissolved fly ash is optionally subjected to washing and drying.
The fly ash used in the alkali dissolution reaction of step (1) may be pulverized coal furnace high-alumina fly ash. The high-alumina fly ash of the pulverized coal furnace is fly ash obtained by collecting coal after the coal is combusted by the pulverized coal furnace and then collected by a dust remover. The coal ash is different in sources of fuel coal used by coal-fired boilers in different areas and different in combustion modes of the boilers, but has the common characteristic that the total content of aluminum element and silicon element is relatively high, and the total content of the aluminum element and the silicon element is generally more than 70% of the total content of the coal ash. In one or more embodiments, the content of aluminum element in the pulverized coal furnace high-alumina fly ash is more than 40 mass%, preferably 50 to 60 mass%, in terms of aluminum oxide. For example, the content of aluminum element in terms of alumina in the pulverized coal furnace high-alumina fly ash may be 40 mass%, 50 mass%, 60 mass%, 70 mass%, 80 mass%, 90 mass%, 100 mass%, or a range defined by any two of the above values.
The kind of the alkali solution used in the alkali leaching reaction of step (1) is not particularly limited in principle, and may be selected according to actual needs by those skilled in the art. In one or more embodiments, the alkali solution used in step (1) is selected from one or more of sodium hydroxide solution, sodium carbonate solution, potassium hydroxide solution, calcium hydroxide solution, barium hydroxide solution, aluminum hydroxide solution, magnesium hydroxide solution, ammonia, preferably sodium hydroxide solution.
In one or more embodiments, the alkaline solution used in the alkaline leaching reaction of step (1) has a mass concentration of 50 to 230g/L, preferably 80 to 150g/L, and more preferably 100 to 130g/L. For example, the mass concentration of the alkaline solution used in step (1) may be 50, 60, 70, 80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, 190, 200, 210, 220, 230g/L or a range defined by any two of the above values.
In one or more embodiments, in the alkali leaching reaction of step (1), the ratio of the volume of the alkali solution to the mass of the fly ash is (1.0-7.0) mL:1g, preferably (2.5-6.0) mL:1g, and more preferably (3.5-5.0) mL:1g. It will be appreciated that when the ratio of the volume of the alkaline solution to the mass of the fly ash is described as, for example, (2.5-6.0) mL:1g, the ratio means mixing in a ratio of 2.5-6.0mL alkaline solution per 1g fly ash or 250-600mL alkaline solution per 100g fly ash or 2.5-6.0L alkaline solution per 1kg fly ash. In exemplary embodiments, the ratio of the volume of the alkaline solution to the mass of the fly ash may be 1.0ml:1g, 1.5ml:1g, 2.0ml:1g, 2.5ml:1g, 3.0ml:1g, 3.5ml:1g, 4.0ml:1g, 4.5ml:1g, 5.0ml:1g, 5.5ml:1g, 6.0ml:1g, 7.0ml:1g, or a range defined by any two of the above values.
In one or more embodiments, in the alkali leaching reaction of step (1), the ratio of the alkali contained in the alkali solution to the mass of the fly ash is (0.1 to 1.0): 1, preferably (0.3 to 0.6): 1. For example, the mass ratio of alkali contained in the alkali solution to the fly ash may be 0.1:1, 0.2:1, 0.3:1, 0.4:1, 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1.0:1, or a range defined by any two of the above values.
In one or more embodiments, the reaction temperature of the alkali dissolution reaction is 60 to 150 ℃, preferably 70 to 110 ℃, and more preferably 80 to 90 ℃. For example, the reaction temperature of the alkali dissolution reaction may be 60, 70, 80, 90, 100, 110, 120, 130, 140, 150 ℃ or a range defined by any two of the above values.
In one or more embodiments, the alkali dissolution reaction has a reaction time of 1 to 10 hours, preferably 2 to 6 hours. For example, the reaction time of the alkali dissolution reaction may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 hours or a range defined by any two of the above values.
The specific manner of solid-liquid separation is not particularly limited, and one skilled in the art may in principle use any suitable solid-liquid separation method known in the art, including but not limited to: centrifugal separation, filtration separation, and the like. In one or more embodiments, the solid-liquid separation in step (1) is performed by filtration, preferably by suction filtration under reduced pressure, for example at a pressure of-0.08 to-0.06 Mpa.
In the step (1), the obtained reaction mixture is subjected to solid-liquid separation to obtain a solid phase and a liquid phase, wherein the solid phase is alkali-dissolved fly ash, and the liquid phase is alkali-dissolved liquid.
Optionally, the alkali-soluble fly ash is subjected to washing and drying for use in a subsequent acid leaching reaction. The manner of washing and drying is not particularly limited, and the person skilled in the art may in principle use any suitable manner known in the art for washing and drying. In one or more embodiments, the alkali-soluble fly ash is washed with water and then dried. The drying may be carried out at a temperature of 90-120 ℃, e.g. 100-105 ℃, e.g. 90, 95, 100, 105, 110, 115, 120 ℃, or a range defined by any two of the above values. The drying time may be greater than or equal to 4 hours, such as 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, or a range defined by any two of the above values.
2. Step (2)
In step (2) an acid solution is provided and one or more of sodium fluoride, potassium fluoride, ammonium fluoride, preferably ammonium fluoride, is added to the acid solution to form an acid leaching solution.
In one or more embodiments, the acid solution in step (2) is selected from one or more of hydrochloric acid solution, sulfuric acid solution, carbonic acid solution, phosphoric acid solution, preferably hydrochloric acid solution.
In one or more embodiments, the mass concentration of the acid solution in step (2) is 5 to 37 mass%, preferably 10 to 30 mass%, further preferably 14 to 25 mass%. For example, the mass concentration of the acid solution in step (2) may be 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37 mass% or a range defined by any two of the above values.
The amount of fluoride contained in the acid leaching solution used in step (3) is related to the amount of alkali-soluble fly ash that needs to be subjected to an acid leaching treatment. In one or more embodiments, the mass of fluoride contained in the acid leaching solution used in step (3) is 1% to 15%, preferably 2% to 10%, further preferably 3% to 5% of the mass of alkali-soluble fly ash used in step (3). For example, the mass of fluoride contained in the acid leaching solution used in step (3) is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15% or a range defined by any two of the above values of the mass of alkali-soluble fly ash used in step (3).
3. Step (3)
In step (3), the alkali-soluble fly ash obtained in step (1) is added to the acid leaching solution formed in step (2), acid leaching reaction is performed, and then the obtained reaction mixture is subjected to solid-liquid separation to obtain acid leached fly ash and acid leaching solution, and the acid leached fly ash is optionally subjected to washing and drying.
In one or more embodiments, in the acid leaching reaction of step (3), the acid leaching solution is heated to 80-200 ℃, and then the alkali-soluble fly ash obtained in step (1) is added thereto to perform the acid leaching reaction. For example, the acid leaching solution may be heated to 80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, 190, 200 ℃ or a range defined by any two of the above values.
In a further preferred manner, the acid leaching solution is heated to 100-180 ℃, more preferably 130-150 ℃, and then the alkali-soluble fly ash obtained in step (1) is added thereto to perform the acid leaching reaction. The applicant found that when the acid leaching solution is heated to the above temperature range, the Ca and Fe contents in the finally obtained aluminum silicon oxide can be further reduced by carrying out the acid leaching reaction at a high temperature in combination with the use of specific fluorides (one or more of sodium fluoride, potassium fluoride, ammonium fluoride).
In one or more embodiments, in the acid leaching reaction of step (3), the ratio of the volume of the acid leaching solution to the mass of the alkali-leached fly ash is (2-20) mL:1g, preferably (4-10) mL:1g, and more preferably (5-8) mL:1g. It will be appreciated that when the ratio of the volume of the acid leaching solution to the mass of the alkali-soluble fly ash is described as, for example, (4-10) mL:1g, the ratio means mixing at a ratio of 4-10mL of the acid leaching solution per 1g of the alkali-soluble fly ash or 400-1000mL of the acid leaching solution per 100g of the alkali-soluble fly ash or 4-10L of the acid leaching solution per 1kg of the alkali-soluble fly ash. In exemplary embodiments, the ratio of the volume of the acid leaching solution to the mass of the alkali-dissolved fly ash may be 2ml:1g, 3ml:1g, 4ml:1g, 5ml:1g, 6ml:1g, 7ml:1g, 8ml:1g, 9ml:1g, 10ml:1g, 11ml:1g, 12ml:1g, 13ml:1g, 14ml:1g, 15ml:1g, 16ml:1g, 17ml:1g, 18ml:1g, 19ml:1g, 20ml:1g, or a range defined by any two of the above values.
In one or more embodiments, in the acid leaching reaction of step (3), the mass ratio of the acid contained in the acid leaching solution to the alkali-leached fly ash is (3.0 to 10.0): 1, preferably (3.0 to 8.0): 1. For example, the mass ratio of acid contained in the acid leaching solution to the alkali-extracted fly ash may be 3.0:1, 3.5:1, 4.0:1, 4.5:1, 5.0:1, 5.5:1, 6.0:1, 6.5:1, 7.0:1, 7.5:1, 8.0:1, 8.5:1, 9.0:1, 9.5:1, 10.0:1, or a range defined by any two of the above values.
In one or more embodiments, the acid leaching reaction has a reaction time of 1 to 10 hours, preferably 2 to 4 hours. For example, the reaction time of the acid leaching reaction may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 hours or a range defined by any two of the above values.
The manner of solid-liquid separation is not particularly limited, and one skilled in the art may in principle use any suitable solid-liquid separation method known in the art, including but not limited to: centrifugal separation, filtration separation, and the like. In one or more embodiments, the solid-liquid separation in step (2) is performed by filtration, preferably by suction filtration under reduced pressure, for example at a pressure of-0.08 to-0.06 Mpa.
In step (3), the resulting reaction mixture is subjected to solid-liquid separation to obtain a solid phase and a liquid phase, wherein the solid phase is acid leached fly ash and the liquid phase is acid leached liquid.
Optionally, the acid leached fly ash is subjected to washing and drying for subsequent calcination treatment. The manner of washing and drying is not particularly limited, and the person skilled in the art may in principle use any suitable manner known in the art for washing and drying. In one or more embodiments, the acid leached fly ash is washed with water and then dried. The drying may be carried out at a temperature of 90-120 ℃, e.g. 100-105 ℃, e.g. 90, 95, 100, 105, 110, 115, 120 ℃, or a range defined by any two of the above values. The drying time may be greater than or equal to 4 hours, such as 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, or a range defined by any two of the above values.
4. Step (4)
In the step (4), roasting the acid leached fly ash obtained in the step (3) to obtain the aluminum silicon oxide. The calcination treatment may be performed in a muffle furnace.
In one or more embodiments, the firing treatment may be at a temperature of 500-1600 ℃, preferably 600-1300 ℃, e.g., 500, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400, 1500, 1600 ℃, or a range defined by any two of the above values.
In one or more embodiments, the firing treatment time may be from 1 to 20 hours, preferably from 1 to 4 hours, for example 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20 hours or a range defined by any two of the above values.
In a preferred embodiment, in the step (4), the acid leached fly ash obtained in the step (3) is washed with water, dried, and then the dried acid leached fly ash is subjected to roasting treatment at 500-1600 ℃ for 1-20 hours, and is cooled to obtain the aluminum silicon oxide.
5. Process flow for preparing aluminum silicon oxide from fly ash
An exemplary embodiment of a method for preparing aluminum silicon oxide using fly ash according to the present invention will be described below with reference to fig. 1. The embodiment shown in fig. 1 is merely illustrative, and embodiments of the present invention are not limited thereto.
Fig. 1 shows a schematic flow chart of a method for preparing aluminum silicon oxide using fly ash according to the present invention.
Firstly, carrying out alkali dissolution treatment on high-alumina fly ash, and then carrying out solid-liquid separation on alkali dissolution reaction products through filtering for example to obtain a solid phase and a liquid phase, wherein the solid phase is one-time alkali dissolution of the fly ash. The obtained primary alkali-eluted fly ash is subjected to acid leaching treatment, and an auxiliary agent (for example, ammonium fluoride) is added to the acid leaching solution. And carrying out solid-liquid separation on the acid leaching reaction product by filtering for example to obtain a solid phase and a liquid phase, wherein the solid phase is the secondary acid leaching fly ash. Roasting the obtained secondary acid leached fly ash, and cooling to obtain the low-iron low-calcium aluminum silicon oxide.
It should be understood that in this specification (including the above and examples section below), the expressions "primary" and "secondary" in "primary alkali leaching" and "secondary acid leaching" are intended to refer only to the relative temporal order of "alkali leaching" and "acid leaching" and are not intended to refer to the number of times "alkali leaching" and "acid leaching" are carried out.
Aluminum silicon oxide
In a second aspect, the present invention relates to an aluminium silicon oxide, obtainable by a process according to the first aspect.
The aluminum silicon oxide prepared by the method has high purity, low impurity content and very high quality.
In one or more embodiments, the aluminum silicon oxide has an elemental iron content in terms of iron oxide of less than 0.40 mass%, preferably less than 0.20 mass%. For example, the aluminum silicon oxide may have less than 0.40 mass%, less than 0.39 mass%, less than 0.38 mass%, less than 0.37 mass%, less than 0.36 mass%, less than 0.35 mass%, less than 0.34 mass%, less than 0.33 mass%, less than 0.32 mass%, less than 0.31 mass%, less than 0.30 mass%, less than 0.29 mass%, less than 0.28 mass%, less than 0.27 mass%, less than 0.26 mass%, less than 0.25 mass%, less than 0.24 mass%, less than 0.23 mass%, less than 0.22 mass%, less than 0.21 mass%, less than 0.20 mass%, less than 0.19 mass%, less than 0.18 mass%, less than 0.17 mass%, less than 0.16 mass%, less than 0.15 mass%, less than 0.14 mass%, less than 0.13 mass%, less than 0.12 mass%, less than 0.11 mass%, less than 0.10 mass%, less than 0.09 mass%, less than 0.08 mass%, less than 0.03 mass%, less than 0.02 mass%, less than 0.03 mass%, less than 0.04 mass%, or less than 0.0.02 mass% iron.
In one or more embodiments, the aluminum silicon oxide has a calcium element content in terms of calcium oxide of less than 0.20 mass%, preferably less than 0.06 mass%. For example, the aluminum silicon oxide may have a calcium element content in terms of calcium oxide of less than 0.20 mass%, less than 0.19 mass%, less than 0.18 mass%, less than 0.17 mass%, less than 0.16 mass%, less than 0.15 mass%, less than 0.14 mass%, less than 0.13 mass%, less than 0.12 mass%, less than 0.11 mass%, less than 0.10 mass%, less than 0.09 mass%, less than 0.08 mass%, less than 0.07 mass%, less than 0.06 mass%, less than 0.05 mass%, less than 0.04 mass%, less than 0.03 mass%, less than 0.02 mass%, or less than 0.01 mass%.
In one or more embodiments, the aluminum silicon oxide has an iron element content of less than 0.40 mass% as iron oxide and a calcium element content of less than 0.20 mass% as calcium oxide, preferably has an iron element content of less than 0.20 mass% as iron oxide and a calcium element content of less than 0.06 mass% as calcium oxide, based on the total mass of the aluminum silicon oxide.
Examples
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Hereinafter, unless otherwise indicated, the mentioned contents or concentrations are by mass.
1. Measurement method
The compositions of the high alumina fly ash, the primary alkali-leached fly ash, the secondary acid-leached fly ash and the aluminum silicon oxide in each of the examples and comparative examples were measured by the following methods:
after the material to be tested is sampled by a glass melting method, the material to be tested is measured by an X-ray fluorescence spectrometer (Siemens 4200), and the specific steps are as follows: uniformly mixing a material to be tested and a fluxing agent (lithium tetraborate) according to a mass ratio of 1:10, placing the mixture into a sample melting furnace, melting the sample at 1050 ℃ for 40min, cooling the mixture to form a glass body with uniform texture, and placing the glass body into an X-ray fluorescence spectrometer for measurement.
2. Raw material source
The sources of the raw materials involved in the examples are shown in table 1 below.
Table 1: sources of the raw materials
3. Preparation and characterization of aluminum silicon oxides
Example 1
The aluminum silicon oxide is prepared from the fly ash by the following steps:
1. preparing 300ml of sodium hydroxide solution with the sodium hydroxide concentration of 100g/L in a 500ml beaker, and heating to 80 ℃;
2. according to 3ml: the liquid-solid ratio of 1g is added with 100g of high-alumina fly ash into the sodium hydroxide solution obtained in the step 1, and stirring reaction is carried out for 2h;
3. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the solid phase of the primary alkali-dissolved fly ash, and the liquid phase of the primary alkali-dissolved fly ash;
4. Preparing 300ml of hydrochloric acid solution with the hydrochloric acid concentration of 15% in a 500ml beaker, adding 3.75g of ammonium fluoride, and heating to 80 ℃;
5. according to 4ml: adding 75g of the primary alkali-dissolved fly ash obtained in the step 3 into the solution obtained in the step 4 according to the liquid-solid ratio of 1g, and stirring for reaction for 2h;
6. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the fly ash with the solid phase being the secondary acid leaching liquid, and the liquid phase being the secondary acid leaching liquid;
7. and (3) placing the secondary acid leached fly ash obtained in the step (6) into a muffle furnace for roasting at 800 ℃ for 1h to obtain the aluminum silicon oxide.
The contents of each element (in oxide form of the corresponding element) in the high alumina fly ash used in step 2, the primary alkali-eluted fly ash obtained in step 3, the secondary acid-eluted fly ash obtained in step 6, and the aluminum silicon oxide obtained in step 7 were measured according to the measurement methods described hereinabove, respectively, and the results are shown in table 2 below:
table 2: composition of high alumina fly ash, primary alkali-leached fly ash, secondary acid-leached fly ash and aluminum silicon oxide in example 1
As is clear from the results in Table 2, fe is contained in the aluminum silicon oxide obtained in example 1 2 O 3 The iron content was 0.27% and the calcium content was 0.08% as CaO.
Example 2
The aluminum silicon oxide is prepared from the fly ash by the following steps:
1. preparing 300ml of sodium hydroxide solution with the sodium hydroxide concentration of 120g/L in a 500ml beaker, and heating to 80 ℃;
2. according to 2.5ml:1.0g of liquid-solid ratio, adding 120g of high-alumina fly ash into the sodium hydroxide solution obtained in the step 1, and stirring for reaction for 2h;
3. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the solid phase of the primary alkali-dissolved fly ash, and the liquid phase of the primary alkali-dissolved fly ash;
4. preparing 300ml of hydrochloric acid solution with the hydrochloric acid concentration of 20% in a 500ml beaker, adding 1.5g of ammonium fluoride, and heating to 80 ℃;
5. according to 6ml: adding 50g of the primary alkali-dissolved fly ash obtained in the step 3 into the solution obtained in the step 4 according to the liquid-solid ratio of 1g, and stirring for reaction for 3h;
6. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the fly ash with the solid phase being the secondary acid leaching liquid, and the liquid phase being the secondary acid leaching liquid;
7. and (3) placing the secondary acid leached fly ash obtained in the step (6) into a muffle furnace for roasting at 800 ℃ for 1h to obtain the aluminum silicon oxide.
The contents of each element (in oxide form of the corresponding element) in the high alumina fly ash used in step 2, the primary alkali-eluted fly ash obtained in step 3, the secondary acid-eluted fly ash obtained in step 6, and the aluminum silicon oxide obtained in step 7 were measured according to the measurement methods described hereinabove, respectively, and the results are shown in table 3 below:
Table 3: composition of high alumina fly ash, primary alkali-leached fly ash, secondary acid-leached fly ash and aluminum silicon oxide in example 2
As is clear from the results in Table 3, fe is contained in the aluminum silicon oxide obtained in example 2 2 O 3 The iron content was 0.29% and the calcium content was 0.07% as CaO.
Example 3
The aluminum silicon oxide is prepared from the fly ash by the following steps:
1. preparing 400ml of sodium hydroxide solution with the sodium hydroxide concentration of 120g/L in a 500ml beaker, and heating to 90 ℃;
2. according to 4ml: the liquid-solid ratio of 1g is added with 100g of high-alumina fly ash into the sodium hydroxide solution obtained in the step 1, and stirring reaction is carried out for 2.5h;
3. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the solid phase of the primary alkali-dissolved fly ash, and the liquid phase of the primary alkali-dissolved fly ash;
4. 400ml of hydrochloric acid solution with the hydrochloric acid concentration of 20% is prepared in a 500ml beaker, 1.5g of ammonium fluoride is added, and the mixture is heated to 90 ℃;
5. according to 8ml: adding 50g of the primary alkali-dissolved fly ash obtained in the step 3 into the solution obtained in the step 4 according to the liquid-solid ratio of 1g, and stirring for reaction for 6h;
6. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the fly ash with the solid phase being the secondary acid leaching liquid, and the liquid phase being the secondary acid leaching liquid;
7. And (3) placing the secondary acid leached fly ash obtained in the step (6) into a muffle furnace for roasting at 800 ℃ for 1h to obtain the aluminum silicon oxide.
The contents of each element (in oxide form of the corresponding element) in the high alumina fly ash used in step 2, the primary alkali-eluted fly ash obtained in step 3, the secondary acid-eluted fly ash obtained in step 6, and the aluminum silicon oxide obtained in step 7 were measured according to the measurement methods described hereinabove, respectively, and the results are shown in table 4 below:
table 4: composition of high alumina fly ash, primary alkali-leached fly ash, secondary acid-leached fly ash and aluminum silicon oxide in example 3
As is clear from the results in Table 4, fe is contained in the aluminum silicon oxide obtained in example 3 2 O 3 The iron content was 0.30% and the calcium content was 0.09% as CaO.
Example 4
The aluminum silicon oxide is prepared from the fly ash by the following steps:
1. preparing 400ml of sodium hydroxide solution with the sodium hydroxide concentration of 130g/L in a 500ml beaker, and heating to 85 ℃;
2. according to 4ml: the liquid-solid ratio of 1g is added with 100g of high-alumina fly ash into the sodium hydroxide solution obtained in the step 1, and stirring reaction is carried out for 4h;
3. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the solid phase of the primary alkali-dissolved fly ash, and the liquid phase of the primary alkali-dissolved fly ash;
4. 400ml of hydrochloric acid solution with the hydrochloric acid concentration of 15% is prepared in a 500ml beaker, 1.5g of ammonium fluoride is added, and the mixture is heated to 85 ℃;
5. according to 8ml: adding 50g of the primary alkali-dissolved fly ash obtained in the step 3 into the solution obtained in the step 4 according to the liquid-solid ratio of 1g, and stirring for reaction for 2h;
6. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the fly ash with the solid phase being the secondary acid leaching liquid, and the liquid phase being the secondary acid leaching liquid;
7. and (3) placing the secondary acid leached fly ash obtained in the step (6) into a muffle furnace for roasting at 800 ℃ for 1h to obtain the aluminum silicon oxide.
The contents of each element (in oxide form of the corresponding element) in the high alumina fly ash used in step 2, the primary alkali-eluted fly ash obtained in step 3, the secondary acid-eluted fly ash obtained in step 6, and the aluminum silicon oxide obtained in step 7 were measured according to the measurement methods described hereinabove, respectively, and the results are shown in table 5 below:
table 5: composition of high alumina fly ash, primary alkali-leached fly ash, secondary acid-leached fly ash and aluminum silicon oxide in example 4
As is clear from the results in Table 5, fe is contained in the aluminum silicon oxide obtained in example 4 2 O 3 The iron content was 0.29% and the calcium content was 0.08% calculated as CaO.
Example 5
The aluminum silicon oxide is prepared from the fly ash by the following steps:
1. preparing 300ml of sodium hydroxide solution with the sodium hydroxide concentration of 100g/L in a 500ml beaker, and heating to 80 ℃;
2. according to 3ml: the liquid-solid ratio of 1g is added with 100g of high-alumina fly ash into the sodium hydroxide solution obtained in the step 1, and stirring reaction is carried out for 2h;
3. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the solid phase of the primary alkali-dissolved fly ash, and the liquid phase of the primary alkali-dissolved fly ash;
4. preparing 300ml of hydrochloric acid solution with the hydrochloric acid concentration of 15% in a 500ml beaker, adding 3.75g of ammonium fluoride, and heating to 150 ℃ by adopting a homogeneous reactor;
5. according to 4ml: adding 75g of the primary alkali-dissolved fly ash obtained in the step 3 into the solution obtained in the step 4 according to the liquid-solid ratio of 1g, and stirring for reaction for 2h;
6. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the fly ash with the solid phase being the secondary acid leaching liquid, and the liquid phase being the secondary acid leaching liquid;
7. and (3) placing the secondary acid leached fly ash obtained in the step (6) into a muffle furnace for roasting at 800 ℃ for 1h to obtain the aluminum silicon oxide.
The contents of each element (in oxide form of the corresponding element) in the high alumina fly ash used in step 2, the primary alkali-eluted fly ash obtained in step 3, the secondary acid-eluted fly ash obtained in step 6, and the aluminum silicon oxide obtained in step 7 were measured according to the measurement methods described hereinabove, respectively, and the results are shown in table 6 below:
Table 6: composition of high alumina fly ash, primary alkali-leached fly ash, secondary acid-leached fly ash and aluminum silicon oxide in example 5
As is clear from the results in Table 6, fe is contained in the aluminum silicon oxide obtained in example 5 2 O 3 The iron content was 0.19% and the calcium content was 0.05% calculated as CaO.
Comparative example 1
The aluminum silicon oxide is prepared from the fly ash by the following steps:
1. preparing 400ml of sodium hydroxide solution with the sodium hydroxide concentration of 120g/L in a 500ml beaker, and heating to 90 ℃;
2. according to 4ml: the liquid-solid ratio of 1g is added with 100g of high-alumina fly ash into the sodium hydroxide solution obtained in the step 1, and stirring reaction is carried out for 2.5h;
3. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the solid phase of the primary alkali-dissolved fly ash, and the liquid phase of the primary alkali-dissolved fly ash;
4. preparing 400ml of hydrochloric acid solution with the hydrochloric acid concentration of 20% in a 500ml beaker, and heating to 90 ℃;
5. according to 8ml: adding 50g of the primary alkali-dissolved fly ash obtained in the step 3 into the solution obtained in the step 4 according to the liquid-solid ratio of 1g, and stirring for reaction for 6h;
6. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the fly ash with the solid phase being the secondary acid leaching liquid, and the liquid phase being the secondary acid leaching liquid;
7. And (3) placing the secondary acid leached fly ash obtained in the step (6) into a muffle furnace for roasting at 800 ℃ for 1h to obtain the aluminum silicon oxide.
The contents of each element (in oxide form of the corresponding element) in the high alumina fly ash used in step 2, the primary alkali-eluted fly ash obtained in step 3, the secondary acid-eluted fly ash obtained in step 6, and the aluminum silicon oxide obtained in step 7 were measured according to the measurement methods described hereinabove, respectively, and the results are shown in the following table 7:
table 7: composition of high alumina fly ash, primary alkali-leached fly ash, secondary acid-leached fly ash and aluminum silicon oxide in comparative example 1
As is clear from the results in Table 7, fe was used as Fe in the aluminum silicon oxide obtained in comparative example 1 2 O 3 The iron content was 0.48% and the calcium content was 0.31% calculated as CaO.
Comparative example 2
The aluminum silicon oxide is prepared from the fly ash by the following steps:
1. preparing 400ml of sodium hydroxide solution with the sodium hydroxide concentration of 130g/L in a 500ml beaker, and heating to 85 ℃;
2. according to 4ml: the liquid-solid ratio of 1g is added with 100g of high-alumina fly ash into the sodium hydroxide solution obtained in the step 1, and stirring reaction is carried out for 4h;
3. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the solid phase of the primary alkali-dissolved fly ash, and the liquid phase of the primary alkali-dissolved fly ash;
4. Preparing 400ml of hydrochloric acid solution with the hydrochloric acid concentration of 15% in a 500ml beaker, and heating to 85 ℃;
5. according to 8ml: adding 50g of the primary alkali-dissolved fly ash obtained in the step 3 into the solution obtained in the step 4 according to the liquid-solid ratio of 1g, and stirring for reaction for 6h;
6. filtering after the reaction is finished, wherein the filtering pressure is-0.08 to-0.06 Mpa, so as to obtain the fly ash with the solid phase being the secondary acid leaching liquid, and the liquid phase being the secondary acid leaching liquid;
7. and (3) placing the secondary acid leached fly ash obtained in the step (6) into a muffle furnace for roasting at 800 ℃ for 1h to obtain the aluminum silicon oxide.
The contents of each element (in oxide form of the corresponding element) in the high alumina fly ash used in step 2, the primary alkali-eluted fly ash obtained in step 3, the secondary acid-eluted fly ash obtained in step 6, and the aluminum silicon oxide obtained in step 7 were measured according to the measurement methods described hereinabove, respectively, and the results are shown in table 8 below:
table 8: composition of high alumina fly ash, primary alkali-leached fly ash, secondary acid-leached fly ash and aluminum silicon oxide in comparative example 2
As is clear from the results in Table 8, in the aluminum silicon oxide obtained in comparative example 2, fe is used as 2 O 3 The iron content was 0.52% and the calcium content was 0.28% calculated as CaO.
Conclusion(s)
From the above results, it is understood that in examples 1 to 5, the addition of the auxiliary agent ammonium fluoride during the acid leaching process produced high-quality aluminum silicon oxide having a low iron content and calcium content, in which the iron content may be less than 0.40 mass% and the calcium content may be less than 0.20 mass%.
Comparative example 1 and example 3 each used an acid leaching reaction time of 6 hours for the preparation of aluminum silicon oxide. However, comparative example 1 differs from example 3 only in that: example 3 the addition of the auxiliary ammonium fluoride during the acid leaching process was performed, whereas comparative example 1 was performed without the addition of ammonium fluoride. Comparing the aluminum silicon oxide compositions obtained in example 3 and comparative example 1 shown in tables 4 and 7, it can be seen that example 3 produced aluminum silicon oxide having significantly lower iron content and calcium content at the same acid leaching reaction time by using an ammonium fluoride aid as compared with comparative example 1.
Comparative example 2 differs from example 4 in that: example 4 an adjuvant ammonium fluoride was added to the acid leaching process and an acid leaching reaction time of only 2 hours was used, whereas comparative example 2 was free of ammonium fluoride and an acid leaching reaction time of 6 hours was used. Comparing the aluminum silicon oxide compositions obtained in example 4 and comparative example 2 shown in tables 5 and 8, it can be seen that example 4 produced aluminum silicon oxide having significantly lower iron content and calcium content by using ammonium fluoride aid with greatly shortened acid leaching reaction time compared to comparative example 2.
Therefore, the above results confirm that when preparing aluminum silicon oxide from fly ash through alkali leaching treatment, acid leaching treatment and roasting treatment, by adding specific fluoride (one or more of sodium fluoride, potassium fluoride, ammonium fluoride, for example, ammonium fluoride) as an auxiliary agent in the acid leaching process, the content of impurities such as iron element, calcium element, etc. in the obtained aluminum silicon oxide can be greatly reduced, while also greatly shortening the acid leaching time.
In addition, example 5 used an elevated acid leaching reaction temperature in combination with the addition of the auxiliary ammonium fluoride during the acid leaching process. Example 5 produced aluminum silicon oxides with further reduced iron and calcium content by using the adjuvant ammonium fluoride in combination with an elevated acid leaching reaction temperature compared to examples 1-4 using a lower acid leaching reaction temperature.
What has been described above is merely an exemplary embodiment of the present invention. It should be noted herein that modifications to the invention can be made by those skilled in the art without departing from the inventive concept, and are intended to be within the scope of the invention.
Claims (36)
1. A process for preparing an aluminum silicon oxide comprising the steps of:
(1) Mixing fly ash with alkali solution, performing alkali dissolution reaction, and then subjecting the obtained reaction mixture to solid-liquid separation to obtain alkali-dissolved fly ash and alkali-dissolved liquid, and optionally subjecting the alkali-dissolved fly ash to washing and drying;
(2) Providing an acid solution, and adding fluoride to the acid solution to form an acid leaching solution, wherein the fluoride is selected from one or more of sodium fluoride, potassium fluoride and ammonium fluoride;
(3) Adding the alkali-soluble fly ash obtained in the step (1) into the acid leaching solution formed in the step (2), performing acid leaching reaction, and then subjecting the obtained reaction mixture to solid-liquid separation to obtain acid leached fly ash and acid leaching solution, and optionally subjecting the acid leached fly ash to washing and drying;
(4) Roasting the acid leached fly ash obtained in the step (3) to obtain aluminum silicon oxide.
2. The method for producing aluminum silicon oxide according to claim 1, wherein the fly ash used in the alkali dissolution reaction of step (1) is pulverized coal furnace high-alumina fly ash in which aluminum element content in terms of aluminum oxide is more than 40 mass%.
3. The method for producing aluminum silicon oxide according to claim 2, wherein the fly ash used in the alkali dissolution reaction of step (1) is pulverized coal furnace high-alumina fly ash in which aluminum element content in terms of aluminum oxide is 50 to 60 mass%.
4. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the alkali solution used in the alkali dissolution reaction of step (1) is selected from one or more of sodium hydroxide solution, sodium carbonate solution, potassium hydroxide solution, calcium hydroxide solution, barium hydroxide solution, aluminum hydroxide solution, magnesium hydroxide solution, aqueous ammonia.
5. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the mass concentration of the alkali solution used in the alkali dissolution reaction of step (1) is 80 to 150g/L.
6. The method for producing aluminum silicon oxide as claimed in claim 5, wherein the alkali solution used in the alkali dissolution reaction of step (1) has a mass concentration of 100 to 130g/L.
7. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein in the alkali dissolution reaction of step (1), the ratio of the volume of the alkali solution to the mass of the fly ash is (2.5 to 6.0) mL:1g.
8. The method for producing aluminum silicon oxide as claimed in claim 7, wherein in the alkali dissolution reaction of step (1), a ratio of a volume of the alkali solution to a mass of the fly ash is (3.5-5.0) mL:1g.
9. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein in the alkali dissolution reaction of step (1), the ratio of the alkali contained in the alkali solution to the mass of the fly ash is (0.1 to 1.0): 1.
10. The method for producing an aluminum silicon oxide as claimed in claim 9, wherein in the alkali dissolution reaction of step (1), a mass ratio of alkali contained in the alkali solution to the fly ash is (0.3 to 0.6): 1.
11. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the reaction temperature of the alkali dissolution reaction is 70 to 110 ℃.
12. The method for preparing aluminum silicon oxide as claimed in claim 11, wherein the reaction temperature of the alkali dissolution reaction is 80-90 ℃.
13. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the reaction time of the alkali dissolution reaction is 1 to 10 hours.
14. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the solid-liquid separation in step (1) and/or (2) is performed by filtration.
15. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the acid solution in step (2) is selected from one or more of hydrochloric acid solution, sulfuric acid solution, carbonic acid solution, phosphoric acid solution.
16. The method for producing aluminum silicon oxide as claimed in claim 15, wherein the acid solution in step (2) is a hydrochloric acid solution.
17. A method for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the mass concentration of the acid solution in step (2) is 5 to 37 mass%.
18. The method for producing aluminum silicon oxide as claimed in claim 17, wherein the mass concentration of the acid solution in step (2) is 10 to 30 mass%.
19. The method for producing aluminum silicon oxide as claimed in claim 17, wherein the mass concentration of the acid solution in step (2) is 14 to 25 mass%.
20. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the mass of the fluoride contained in the acid leaching solution used in step (3) is 1% to 15% of the mass of the alkali-soluble fly ash used in step (3).
21. The method for producing aluminum silicon oxide as claimed in claim 20, wherein the mass of the fluoride contained in the acid leaching solution used in step (3) is 2 to 10% of the mass of the alkali-soluble fly ash used in step (3).
22. The method for producing aluminum silicon oxide as claimed in claim 20, wherein the mass of the fluoride contained in the acid leaching solution used in step (3) is 3% -5% of the mass of the alkali-soluble fly ash used in step (3).
23. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein in the acid leaching reaction of step (3), the ratio of the volume of the acid leaching solution to the mass of the alkali-soluble fly ash is (2 to 20) mL:1g.
24. The method for producing aluminum silicon oxide as claimed in claim 23, wherein in the acid leaching reaction of step (3), a ratio of a volume of the acid leaching solution to a mass of the alkali-soluble fly ash is (4-10) mL:1g.
25. The method for producing aluminum silicon oxide as claimed in claim 23, wherein in the acid leaching reaction of step (3), a ratio of a volume of the acid leaching solution to a mass of the alkali-soluble fly ash is (5-8) mL:1g.
26. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein in the acid leaching reaction of step (3), the mass ratio of the acid contained in the acid leaching solution to the alkali-leached fly ash is (3.0 to 10.0): 1.
27. The method for producing an aluminum silicon oxide as claimed in claim 26, wherein in the acid leaching reaction of step (3), a mass ratio of the acid contained in the acid leaching solution to the alkali-leached fly ash is (3.0 to 8.0): 1.
28. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein in step (3), the acid leaching solution is heated to 80 to 200 ℃ and then the alkali-soluble fly ash obtained in step (1) is added thereto to perform an acid leaching reaction.
29. The process for producing aluminum silicon oxide as claimed in claim 28, wherein in step (3), the acid leaching solution is heated to 100 to 180 ℃ and then the alkali-soluble fly ash obtained in step (1) is added thereto to perform an acid leaching reaction.
30. The method for producing aluminum silicon oxide as claimed in claim 28, wherein in step (3), the acid leaching solution is heated to 130 to 150 ℃ and then the alkali-soluble fly ash obtained in step (1) is added thereto to perform an acid leaching reaction.
31. A process for preparing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the reaction time of the acid leaching reaction is 1 to 10 hours.
32. The process for preparing aluminum silicon oxide as claimed in claim 31, wherein the reaction time of the acid leaching reaction is 2 to 4 hours.
33. A process for producing an aluminum silicon oxide as claimed in any one of claims 1 to 3, wherein the acid leached fly ash obtained in the step (3) is subjected to a roasting treatment at 500 to 1600 ℃ for 1 to 20 hours, and cooled to obtain the aluminum silicon oxide.
34. An aluminum silicon oxide produced according to the method of any one of claims 1 to 33.
35. The aluminum silicon oxide as set forth in claim 34, having an iron element content of less than 0.40 mass% in terms of iron oxide and a calcium element content of less than 0.20 mass% in terms of calcium oxide, based on the total mass of the aluminum silicon oxide.
36. The aluminum silicon oxide as set forth in claim 35 having an iron element content of less than 0.20 mass% in terms of iron oxide and a calcium element content of less than 0.06 mass% in terms of calcium oxide, based on the total mass of the aluminum silicon oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310486528.3A CN116216731B (en) | 2023-05-04 | 2023-05-04 | Method for preparing aluminum silicon oxide by using fly ash and obtained aluminum silicon oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310486528.3A CN116216731B (en) | 2023-05-04 | 2023-05-04 | Method for preparing aluminum silicon oxide by using fly ash and obtained aluminum silicon oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116216731A true CN116216731A (en) | 2023-06-06 |
| CN116216731B CN116216731B (en) | 2023-08-08 |
Family
ID=86585802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310486528.3A Active CN116216731B (en) | 2023-05-04 | 2023-05-04 | Method for preparing aluminum silicon oxide by using fly ash and obtained aluminum silicon oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116216731B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4362703A (en) * | 1982-03-01 | 1982-12-07 | Iowa State University Research Foundation, Inc. | Process for preparing cryolite from fly ash |
| CN111606339A (en) * | 2020-05-22 | 2020-09-01 | 内蒙古蒙泰集团有限公司 | Method for preparing aluminum-silicon oxide by using fly ash |
| CN114940507A (en) * | 2022-06-22 | 2022-08-26 | 神华准能资源综合开发有限公司 | Method for extracting alumina from fly ash |
| CN116040670A (en) * | 2023-03-31 | 2023-05-02 | 内蒙古蒙泰集团有限公司 | Method for producing polyaluminum chloride in process of preparing aluminum silicon oxide from fly ash |
-
2023
- 2023-05-04 CN CN202310486528.3A patent/CN116216731B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4362703A (en) * | 1982-03-01 | 1982-12-07 | Iowa State University Research Foundation, Inc. | Process for preparing cryolite from fly ash |
| CN111606339A (en) * | 2020-05-22 | 2020-09-01 | 内蒙古蒙泰集团有限公司 | Method for preparing aluminum-silicon oxide by using fly ash |
| CN114940507A (en) * | 2022-06-22 | 2022-08-26 | 神华准能资源综合开发有限公司 | Method for extracting alumina from fly ash |
| CN116040670A (en) * | 2023-03-31 | 2023-05-02 | 内蒙古蒙泰集团有限公司 | Method for producing polyaluminum chloride in process of preparing aluminum silicon oxide from fly ash |
Non-Patent Citations (2)
| Title |
|---|
| 孙秀君;舒新前;: "酸浸法提取粉煤灰中氧化铝溶出规律的研究", 无机盐工业, no. 11, pages 44 - 46 * |
| 杨慧芬;孟家乐;张伟豪;宋荣龙;江波;: "盐酸-氢氟酸对高铝粉煤灰中铝的浸出作用", 无机盐工业, no. 03, pages 43 - 46 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116216731B (en) | 2023-08-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7871583B2 (en) | Process for recovery of silica followed by alumina from coal fly ash | |
| CN101293663B (en) | Novel technique for preparing fine calcium carbonate | |
| CN102167338B (en) | Technology for preparing hydrated sodium aluminosilicate by utilizing high-alumina coal gangue and fly ash alkali soluble desiliconization | |
| CN110372236A (en) | A kind of Desulphurization prepares method of alpha semi-hydrated gypsum and products thereof | |
| CN111606339B (en) | Method for preparing aluminum-silicon oxide by using fly ash | |
| CN102586610A (en) | Cleaner production process for synchronously extracting vanadium and aluminum from aluminothermic vanadium iron slag | |
| CN105967201A (en) | Method for producing P-type zeolite from fly ash acid sludge | |
| CN102838147B (en) | Method for preparing mixed solution of sodium aluminate and potassium aluminate from alkaline syenite | |
| CN115216645A (en) | Method for extracting lithium from electrolytic aluminum waste slag by mixed salt calcination method | |
| CN106745027A (en) | A kind of flyash synthesizes the method for analcime | |
| CN1384214A (en) | Carbon reducting roast process of producing RE chloride with mixed RE concentrate | |
| CN106966415A (en) | The process of aluminum oxide in a kind of acidity extraction coal-powder boiler flyash | |
| CN107129169A (en) | A kind of preparation method of magnesium oxysulfide concrete | |
| CN109402380A (en) | A method of the vanadium extraction from vanadium slag | |
| CN106241873A (en) | The preparation method of high-purity vanadium pentoxide | |
| CN116216731B (en) | Method for preparing aluminum silicon oxide by using fly ash and obtained aluminum silicon oxide | |
| CN110844928A (en) | Method for preparing micro-nano aluminum oxide from aluminum alloy hydrolysate | |
| CN102732727B (en) | Method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag | |
| CN100387524C (en) | Method of preparing rare earth fluoride from rare earth oxide | |
| CN104891504B (en) | A kind of method for extracting white carbon from cinder | |
| WO2020195721A1 (en) | Spinel powder | |
| JP6080980B2 (en) | Preparation of silica-alumina composition | |
| CN108516565A (en) | A method of preparing P type zeolite molecular sieve using aluminium calcium powder reaction slag | |
| CN109231247A (en) | A kind of method that the by-product of fluosilicic acid legal system aluminum fluoride prepares ice crystal | |
| CN107619952B (en) | A method of leaching lithium from flyash |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |