CN115465869A - Method for preparing calcium iron polysilicate from gasified slag - Google Patents
Method for preparing calcium iron polysilicate from gasified slag Download PDFInfo
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- CN115465869A CN115465869A CN202211347523.4A CN202211347523A CN115465869A CN 115465869 A CN115465869 A CN 115465869A CN 202211347523 A CN202211347523 A CN 202211347523A CN 115465869 A CN115465869 A CN 115465869A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
Abstract
The invention discloses a method for preparing polysilicate aluminum, iron and calcium silicate by using gasified slag, which is implemented by the following steps: step 1, placing gasified slag in an oven for drying, crushing by a crusher and sieving for later use; step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 2% -25% of the mass of the gasified slag; step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 5% -10% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after full acid leaching to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:5-1; step 4, regulating the pH value of the pickle liquor to 3-5 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the calcium iron polysilicate after full reaction; and 5, carrying out solid-liquid separation on the crude product of the polyaluminium silicate iron calcium, drying, crushing and sieving to obtain a finished product of the polyaluminium silicate iron calcium.
Description
Technical Field
The invention belongs to the technical field of coal-based solid waste resource treatment, and particularly relates to a method for preparing poly-aluminum-ferric-calcium silicate by gasifying slag.
Background
The gasified slag is an industrial byproduct of the coal gasification process. The chemical compositions of the gasified slag are different from one region to another due to different coal chemical component contents in different regions. According to incomplete statistics, the gas slagging output exceeds 6000 million tons/year. The treatment modes of enterprises in various regions for the gasified slag are outward transportation, landfill, open stacking and the like, and the treatment modes have the disadvantages of increasing the enterprise cost, polluting the soil, easily causing the PM2.5 in the air to exceed the standard and the like, and seriously threaten the health and safety of people.
The aluminum-iron-calcium polysilicate flocculant has the advantages of strong flocculation capacity, high water purification efficiency, easy transportation and storage, good water solubility and wide pH application range (5.0-9.0), and is a novel high-efficiency inorganic polymeric flocculant. The key of the production cost of the aluminum-iron-calcium polysilicate flocculant is the raw material source. At present, the conventional method for preparing the polyaluminium silicate iron calcium flocculant is to use iron ore, bauxite and limestone as sources, add substances capable of generating silicic acid, such as sodium silicate, and adjust the pH value and then carry out polymerization reaction to obtain the polyaluminium silicate iron calcium flocculant. The resources of iron ore, aluminum ore and the like are increasingly tense, and the preparation of the polyaluminium silicate iron calcium by taking the iron ore, the aluminum ore and the like as raw materials is not beneficial to long-term sustainable development. And the traditional iron ore and aluminum ore treatment process has the defects of complex process, high process energy consumption, high cost, easy secondary pollution and the like.
The invention provides a process for synthesizing the calcium iron polysilicate by one step by using coal gasification solid waste coal gasification slag as a raw material. The process has the advantages of wide raw material source, large total amount and low cost, and the produced polysilicate aluminum iron calcium has wide profit margin and wide market demand.
Disclosure of Invention
The invention aims to provide a method for preparing polyaluminium silicate iron calcium by using coal gasification slag.
In order to achieve the purpose, the invention adopts the technical scheme that the method for preparing the polyaluminium silicate iron calcium by gasifying the slag is characterized by comprising the following steps of: the method is implemented according to the following steps:
step 1, placing the gasified slag in a drying oven for drying, crushing by a crusher and sieving for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 2% -25% of the mass of the gasified slag;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 5% -10% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after full acid leaching to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:5-1;
step 4, regulating the pH of the pickle liquor to 3-5 by hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the aluminum-iron-calcium polysilicate after full reaction;
and 5, carrying out solid-liquid separation on the crude product of the polyaluminium silicate iron calcium, drying, crushing and sieving to obtain a finished product of the polyaluminium silicate iron calcium.
As a preferable technical scheme of the invention, in the step 1, the gasified slag is dried in an oven at the temperature of 80-100 ℃ for 12-24 h.
In the step 1, the crushing time is 10-15 s, and the powder is sieved by a 100-200-mesh sieve.
As a preferred embodiment of the present invention, in the step 2, the muffle furnace calcination operation is: raising the temperature to 800-1000 ℃ at a constant rate, and keeping the temperature for 0.5-1 h.
As a preferable technical scheme of the invention, in the step 3, the temperature of stirring and heating is 60-100 ℃, the rotation speed of stirring is 160-480 r/min, and the time of acid leaching reaction is 1-5 h.
In a preferred embodiment of the present invention, in the step 4, the time for heating to the polymerization temperature is 1h to 6h in the hydrochloric acid solution with acid and alkali content of 0.1M to 1.0M and the sodium hydroxide solution with alkali content of 0.1M to 1.0M.
As a preferable technical scheme of the invention, in the step 5, the crude poly aluminum silicate iron calcium obtained in the step 4 is subjected to solid-liquid separation, dried in an oven at 80-100 ℃ for 12-24 h, crushed in a crusher for 10-15 s, and sieved with a 100-200-mesh sieve to obtain a finished poly aluminum silicate iron calcium product.
The invention has the beneficial effects that: (1) According to the method for preparing the polyaluminium silicate iron calcium from the gasified slag, the selected gasified slag contains rich silicon source, iron source, aluminum source and calcium source, the gasified slag can be efficiently utilized, and the harm to enterprises and the environment caused by the large stacking of the gasified slag is reduced; (2) According to the method for preparing the polyaluminium silicate iron calcium by using the gasified slag, the selected gasified slag contains other metal elements such as calcium, magnesium and the like, and the produced polyaluminium silicate iron calcium contains metal ions such as calcium, magnesium and the like, so that the polyaluminium silicate iron calcium has a better water purifying effect when being applied to water treatment. (3) The method for preparing the polyaluminium silicate iron calcium by using the gasified slag has the advantages of simple preparation process, cheap raw materials, low process cost and high operation flexibility, does not need to supplement a silicon source, an iron source, an aluminum source and a calcium source in the process of producing the polyaluminium silicate iron calcium, relieves the exhaustion of high-quality bauxite and iron ore resources in China, and has good effect and wide market prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the method for preparing calcium iron polysilicate from gasified slag.
Detailed Description
As shown in figure 1, the method for preparing the calcium iron polysilicate by using the gasified slag comprises the following steps:
step 1, placing the gasified slag in a drying oven at 80-100 ℃ for drying for 12-24 h, crushing for 10-15 s by a crusher, and then sieving by a 100-200-mesh sieve for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 2% -25% of the mass of the gasified slag; the specific calcining method in the muffle furnace comprises the following steps: heating to 800-1000 ℃ at a constant rate, and keeping the temperature for 0.5-1 h;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 5% -10% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after acid leaching for 1-5 h to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:5-1; the stirring and heating temperature is 60-100 ℃, the stirring rotating speed is 160-480 r/min, and the acid leaching reaction time is 1-5 h;
step 4, regulating the pH value of the pickle liquor to 3-5 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the calcium iron polysilicate after full reaction; hydrochloric acid solution with acid and alkali of 0.1-1.0M and sodium hydroxide solution with alkali of 0.1-1.0M, and heating to polymerization temperature for 1-6 h;
and 5, performing solid-liquid separation on the crude poly aluminum silicate iron calcium obtained in the step 4, drying in an oven at the temperature of 80-100 ℃ for 12-24 h, crushing in a crusher for 10-15 s, and sieving with a 100-200-mesh sieve to obtain a finished poly aluminum silicate iron calcium product.
And (3) performing flocculation decolorizing performance test on the prepared polysilicate aluminum iron calcium. The sewage used for flocculation is landfill leachate with pH =8, and the specific flocculation process is as follows: 100mg of calcium iron polysilicate was dissolved in 50ml of water with stirring. 100ml of landfill leachate is added into a 250ml beaker, after magnetic stirring is carried out for 30 seconds (300 rpm), a certain amount of aluminum-iron-calcium polysilicate solution is added by a dropper, the mixture is rapidly stirred (200 rpm) for 1 minute and slowly stirred (40 rpm) for 10 minutes, and after standing and precipitating for 30 minutes, a supernatant liquid at the position 2cm below the liquid surface is taken for analysis.
Determination of decolorization removal rate: and (3) measuring the decoloring performance of the flocculant by adopting an absorbance method, and using deionized water as a blank sample. Firstly, scanning a water sample before treatment in the wavelength range of 190-600nm to obtain the maximum absorption wavelength of the sample, and recording the absorbance A of the sample 0 . The supernatant was taken from the treated water sample, and the absorbance A at the maximum absorption wavelength was measured. The chroma removal rate is calculated as follows:
chroma removal rate = (a) 0 -A)/A
The removal rate of the chromaticity of the landfill leachate with the pH =8 of the obtained calcium iron aluminum polysilicate is verified to be 0.65-0.90.
Example 1
The invention relates to a method for preparing polysilicate aluminum, iron and calcium silicate by using gasified slag, which is implemented by the following steps:
step 1, drying the coal gasification slag in an oven at 80 ℃ for 12 hours, crushing for 10 seconds by a crusher, and then sieving by a 200-mesh sieve for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 2% of the mass of the gasified slag; the muffle furnace calcination method specifically comprises the following steps: heating to 800 ℃ at a constant rate, and keeping the temperature for 1h;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 5% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after acid leaching for 1h to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:5; stirring and heating at 60 ℃, stirring at the rotating speed of 160r/min, and performing acid leaching reaction for 1h;
step 4, regulating the pH value of the pickle liquor to 3 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the polysilicate aluminum iron calcium after full reaction; hydrochloric acid solution with acid and alkali of 0.1M and sodium hydroxide solution with alkali of 0.1M, and heating to the polymerization temperature for 6h;
and 5, performing solid-liquid separation on the crude poly aluminum silicate iron calcium obtained in the step 4, drying in an oven of 80-80 ℃ for 12h, crushing in a crusher for 15s, and sieving with a 200-mesh sieve to obtain a finished poly aluminum silicate iron calcium.
Example 2
The invention relates to a method for preparing calcium iron polysilicate by gasifying slag, which is implemented by the following steps:
step 1, drying the gasified slag in a drying oven at 100 ℃ for 12 hours, crushing for 10s by a crusher, and sieving by a 100-mesh sieve for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 25% of the mass of the gasified slag; the specific calcining method in the muffle furnace comprises the following steps: raising the temperature to 1000 ℃ at a constant speed, and keeping the temperature for 0.5h;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 10% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after acid leaching for 5 hours to obtain acid leaching liquid, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1; stirring and heating at 100 deg.C, stirring at 480r/min, and acid leaching for 1h;
step 4, regulating the pH value of the pickle liquor to 5 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the polysilicate aluminum iron calcium after full reaction; 1.0M hydrochloric acid solution and 1.0M sodium hydroxide solution, and heating to the polymerization temperature for 1h;
and 5, performing solid-liquid separation on the crude poly aluminum silicate iron calcium obtained in the step 4, drying in a drying oven at 100 ℃ for 12 hours, crushing for 10 seconds in a crusher, and sieving by using a 100-mesh sieve to obtain a finished poly aluminum silicate iron calcium.
Example 3
The invention relates to a method for preparing polysilicate aluminum, iron and calcium silicate by using gasified slag, which is implemented by the following steps:
step 1, drying the gasified slag in a 90 ℃ oven for 16h, crushing for 13s by a crusher, and then sieving by a 150-mesh sieve for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 13% of the mass of the gasified slag; the specific calcining method in the muffle furnace comprises the following steps: heating to 900 ℃ at a constant speed, and keeping the temperature for 0.7h;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 7% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after acid leaching for 3 hours to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:7; the stirring and heating temperature is 80 ℃, the stirring rotating speed is 320r/min, and the acid leaching reaction time is 3h;
step 4, regulating the pH value of the pickle liquor to 4 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the polysilicate aluminum iron calcium after full reaction; hydrochloric acid solution with acid and alkali of 0.5M and sodium hydroxide solution with alkali of 0.5M, and heating to the polymerization temperature for 4h;
and 5, performing solid-liquid separation on the crude poly aluminum silicate iron calcium obtained in the step 4, drying in a 90 ℃ oven for 18h, crushing for 13s in a crusher, and sieving with a 150-mesh sieve to obtain a finished poly aluminum silicate iron calcium.
Example 4
The invention relates to a method for preparing polysilicate aluminum, iron and calcium silicate by using gasified slag, which is implemented by the following steps:
step 1, drying the coal gasification slag in a drying oven at 85 ℃ for 16h, crushing for 13s by a crusher, and then sieving by a 140-mesh sieve for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 18% of the mass of the gasified slag; the specific calcining method in the muffle furnace comprises the following steps: heating to 850 ℃ at a constant speed, and keeping the temperature for 0.8h;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 9% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after acid leaching for 2 hours to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:9; the stirring and heating temperature is 650 ℃, the stirring rotating speed is 280r/min, and the acid leaching reaction time is 4 hours;
step 4, regulating the pH value of the pickle liquor to 4 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the polysilicate aluminum iron calcium after full reaction; hydrochloric acid solution with acid and alkali of 0.8M and sodium hydroxide solution with alkali of 0.7M, and heating to the polymerization temperature for 2h;
and 5, performing solid-liquid separation on the crude poly aluminum silicate iron calcium obtained in the step 4, drying in an oven at the temperature of 80 ℃ for 20 hours, crushing for 11 seconds in a crusher, and sieving by using a 180-mesh sieve to obtain a finished poly aluminum silicate iron calcium.
Example 5
The invention relates to a method for preparing calcium iron polysilicate by gasifying slag, which is implemented by the following steps:
step 1, drying the gasified slag in a 95 ℃ oven for 14h, crushing for 12s by a crusher, and then sieving by a 170-mesh sieve for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 19% of the mass of the gasified slag; the muffle furnace calcination method specifically comprises the following steps: heating to 950 ℃ at a constant rate, and keeping the temperature for 0.8h;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 10% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after acid leaching for 4 hours to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:6; the stirring and heating temperature is 75 ℃, the stirring rotating speed is 300r/min, and the acid leaching reaction time is 4h;
step 4, regulating the pH value of the pickle liquor to 5 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the polysilicate aluminum iron calcium after full reaction; hydrochloric acid solution with acid and alkali of 0.9 and sodium hydroxide solution with alkali of 0.9M, and the time for heating to the polymerization temperature is 5ha;
and 5, performing solid-liquid separation on the crude poly aluminum silicate iron calcium obtained in the step 4, drying in an oven at 85 ℃ for 18h, crushing for 14s in a crusher, and sieving with a 180-mesh sieve to obtain a finished poly aluminum silicate iron calcium.
Claims (7)
1. A method for preparing polysilicate aluminum, iron and calcium by coal gasification slag is characterized by comprising the following steps: the method is implemented according to the following steps:
step 1, placing gasified slag in an oven for drying, crushing by a crusher and sieving for later use;
step 2, placing the gasified slag and a fluxing agent into a muffle furnace for calcining to obtain solid slag, wherein the fluxing agent accounts for 2% -25% of the mass of the gasified slag;
step 3, mixing the solid residue obtained in the step 2 with hydrochloric acid with the concentration of 5% -10% in a reaction kettle, then heating and stirring, carrying out solid-liquid separation after full acid leaching to obtain acid leaching solution, wherein the solid-liquid ratio of the solid residue to the hydrochloric acid is 1:5-1;
step 4, regulating the pH value of the pickle liquor to 3-5 by using hydrochloric acid or alkali liquor, heating to the polymerization temperature, and obtaining a crude product of the calcium iron polysilicate after full reaction;
and 5, carrying out solid-liquid separation on the coarse product of the polyaluminium silicate iron calcium, drying, crushing and sieving to obtain a finished product of the polyaluminium silicate iron calcium.
2. The method for preparing the calcium iron polysilicate by the gasified slag according to the claim 1, wherein in the step 1, the gasified slag is dried in an oven at 80-100 ℃ for 12-24 h.
3. The method for preparing the calcium iron polysilicate by the coal gasification slag as claimed in claim 2, wherein in the step 1, the crushing time is 10s-15s, and the calcium iron polysilicate is sieved by a 100-200-mesh sieve.
4. The method for preparing the polyaluminium silicate iron calcium by the gasified slag according to the claim 3, wherein in the step 2, the calcining in a muffle furnace is specifically as follows: raising the temperature to 800-1000 ℃ at a constant rate, and keeping the temperature for 0.5-1 h.
5. The method for preparing the polyaluminium silicate iron calcium by the coal gasification slag as claimed in claim 4, wherein in the step 3, the stirring and heating temperature is 60-100 ℃, the stirring rotation speed is 160-480 r/min, and the acid leaching time is 1-5 h.
6. The method for preparing the polyaluminum ferric silicate calcium from the gasified slag according to claim 5, wherein in the step 4, the hydrochloric acid solution with acid and alkali of 0.1M-1.0M and the sodium hydroxide solution with alkali of 0.1M-1.0M are heated to the polymerization temperature for 1h-6h.
7. The method for preparing the calcium iron polysilicate by gasifying the slag according to claim 6, wherein in the step 5, the crude product of the calcium iron polysilicate obtained in the step 4 is subjected to solid-liquid separation, is dried in an oven at 80-100 ℃ for 12-24 h, is crushed for 10-15 s in a crusher, and is sieved by a 100-200-mesh sieve to obtain the finished product of the calcium iron polysilicate.
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