CN109809419B - Method for preparing polysilicate aluminum ferric flocculant - Google Patents
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Abstract
The invention discloses a method for preparing a polymeric ferric aluminum silicate flocculant, which takes industrial solid wastes such as coal gangue, fly ash and red mud as raw materials and is prepared and produced by the steps of raw material preparation, clinker firing, water quenching, crude product water washing separation, inorganic acid regulation, alkali washing and the like. The invention reduces the cost, saves the resources, realizes the cyclic utilization of the activating agent, effectively avoids the environmental pollution, has simple process flow, low energy consumption and simple equipment corrosion problem, and is beneficial to industrialized popularization.
Description
Technical Field
The invention relates to the field of resource utilization of solid wastes such as coal gangue, fly ash and red mud, in particular to a method for preparing a polyaluminum ferric silicate flocculant.
Background
In recent years, along with the rapid development of economic society of China, the discharge amount of urban and industrial wastewater is increased, and the water resource of China is in short supply, so that the discharged wastewater is required to be effectively purified and recycled.
Polyaluminum ferric silicate (PSAF) is a novel water-soluble polyelectrolyte. It is mainly used for purifying drinking water, and can also be used for special water quality treatment of water supply, removing cadmium, fluorine, radioactive contamination, floating oil, etc. Also used for treating industrial wastewater, such as printing and dyeing wastewater, and the like, and also has wide application in the aspects of casting, papermaking, medicine, leather making, and the like. The novel biological sewage treatment agent has an instant effect on sewage treatment in the field of sewage treatment, and is a very popular sewage treatment agent at present. The polymeric aluminum ferric silicate has the characteristics of high ion degree, high water solubility (completely dissolved in water in the whole PH value range and free from the influence of low water temperature), no gel formation, good hydrolytic stability and the like, and is an ideal sewage treatment agent.
SiO in coal gangue, fly ash and red mud2、Al2O3、Fe2O3Chemical components are main raw materials for preparing the polymeric aluminum ferric silicate. And the coal gangue, the fly ash and the red mud are discharged as solid wastes for a long time, so that not only is the resource waste caused, but also a large amount of land is occupied, and double damage is caused to the ecology and the environment. Therefore, the solid wastes such as coal gangue, fly ash and red mud are effectively recycled to prepare the sewage purifying agent, so that the cost is saved, and the method has great practical significance and long-term strategic significance for saving resources, improving the environment and improving the economic and social benefits.
Disclosure of Invention
The invention provides a method for preparing a polyaluminum ferric silicate flocculant, which aims to perform resource utilization on industrial solid wastes such as coal gangue, fly ash and red mud and prepare the polyaluminum ferric silicate flocculant with high added value, thereby saving resources, reducing cost and improving environment.
The object of the invention is achieved in the following technical solutions, however, the invention can be embodied in different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Unless defined otherwise, all 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 terminology used in the description presented herein is for the purpose of describing particular embodiments and is not intended to be limiting. As used in this specification and the appended claims, the singular forms "a", "an", "the" and the like include plural referents unless the context clearly dictates otherwise.
In one aspect, the invention provides a preparation method of a polymeric aluminum ferric silicate flocculant, which is characterized by comprising the following steps: the method for preparing the polyaluminum ferric silicate flocculant by using one or more of coal gangue, fly ash and red mud as raw materials comprises the following steps:
(1) one or more of coal gangue, fly ash and red mud is crushed to more than 100 meshes by a ball mill to be used as a mixed raw material, wherein the ratio of Si/Al/Fe in the mixed raw material is 5-30/20-50/10-40;
(2) uniformly mixing the mixed raw material in the step (1) with an activating agent to prepare a raw material, wherein the activating agent is ammonium sulfate or ammonium chloride or a mixture of the ammonium sulfate and the ammonium chloride, and the mass ratio of the activating agent to the mixed raw material is (5-10): 1;
(3) roasting the raw material in the step (2) at 500-750 ℃ for 1-3 h, wherein the reaction pressure is 0.25-0.3 MPa, so as to obtain clinker and tail gas, carrying out heat exchange on the tail gas, and then, carrying out the next process step, wherein hot gas obtained after heat exchange is used for the next concentration and crystallization step of the solution;
(4) transferring the clinker obtained in the step (3) to water with the same mass for water quenching to obtain a crude product with the particle size of 10-100 microns, wet-grinding the crude product, adding water with the volume being 3 times that of the crude product, fully stirring for 2 hours at 90 ℃, and then carrying out solid-liquid separation to obtain a filtrate A and a filter residue B;
(5) adding hydrogen peroxide with the concentration of 30% into the filtrate A, then introducing tail gas subjected to heat exchange in the step (3), stirring for 1h at 40 ℃ after the reaction is finished, and performing solid-liquid separation to obtain a filtrate C and a filter cake D, wherein the filtrate C is used as an activating agent in the step (2) for recycling after being concentrated and crystallized;
(6) fully mixing calcium aluminate with the filter cake D, adding inorganic acid, stirring and reacting for 4 hours at the temperature of 60-80 ℃, and standing for 2 hours after the reaction is finished to obtain a solution E;
(7) crushing the filter residue B, transferring the crushed filter residue B into a corrosion-resistant high-pressure reaction kettle containing a sodium hydroxide solution, heating to 130 ℃, stirring for reaction for 4 hours, cooling to room temperature, and carrying out solid-liquid separation to obtain a solution F;
(8) mixing the solution E with a solvent according to the mass ratio of (1-1.5): 1 is slowly added into the solution F at a stirring speed of not less than 150 rpm and a reaction temperature of 40 ℃, the pH value of the solution C is adjusted to 3.5-4 by adding inorganic acid after the solution C is added, and the solution C is kept stand for 6-12 hours to obtain the polymeric aluminum ferric silicate flocculant.
Preferably, the tail gas in the step (3) is subjected to two stages of heat exchange processes, medium-high temperature hot gas at 300-350 ℃ is obtained after the first stage of process, medium-high temperature hot gas at 100-150 ℃ is obtained after the second stage of process, and the medium-high temperature hot gas and the medium-temperature hot gas are used in the concentration and crystallization process of the filtrate C in the step (5).
Preferably, the mass of the calcium aluminate in the step (6) is 2-5% of the mass of the filter cake D.
Preferably, inorganic acid is added in the step (6) and the pH value is adjusted to 2.2-2.5.
Preferably, the inorganic acid in the step (6) and the step (8) is 3-10% of industrial hydrochloric acid or 5-15% of industrial sulfuric acid or a mixture of the two.
Preferably, Na in the sodium hydroxide solution in the step (7)2O and SiO in filter residue B2The mass ratio of (A) to (B) is controlled to be 1: (0.6-0.8).
In another aspect, the invention also provides a polymeric ferric aluminum silicate flocculant, which is prepared and produced by the method.
Compared with the prior art, the invention effectively utilizes SiO in industrial solid wastes such as coal gangue, fly ash and red mud2、Al2O3、Fe2O3The polymeric aluminum ferric silicate flocculant is prepared from chemical components, so that the cost is reduced, the resource is saved, and the environmental pollution is effectively avoided. In addition, the method has the advantages of simple process flow, low energy consumption and simple equipment corrosion problem, and is favorable for industrial popularization.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Example 1
The coal gangue, the fly ash and the red mud are mixed in a ratio of 1:1:1.5 to serve as a mixed raw material, wherein the ratio of Si/Al/Fe in the mixed raw material is 30/40/30, and other components such as Ca, Mg, Na, K, Ti and the like can be contained in the mixed raw material, which cannot be used for limiting the protection scope of the invention.
Taking 1000g of the mixed raw materials, ball-milling and crushing the mixed raw materials to more than 100 meshes, and uniformly mixing the mixed raw materials with an activating agent to prepare a raw material, wherein the activating agent is ammonium chloride, and the mass ratio of the activating agent to the mixed raw materials is 7: 1; transferring the prepared raw material to a roasting furnace to roast at 650 ℃, wherein the reaction pressure is 0.3MPa, and roasting is carried out for 2h to obtain clinker and tail gas; cooling the tail gas through two stages of heat exchange procedures, wherein medium-high temperature hot gas at 300-350 ℃ is obtained after the first stage procedure, medium-temperature hot gas at 100-150 ℃ is obtained after the second stage procedure, and the medium-high temperature hot gas and the medium-temperature hot gas are used for the subsequent concentration and crystallization step of the solution; transferring the clinker into 1.5L of water for water quenching to obtain a crude product with the particle size of 10-100 mu m, wet-grinding the crude product, adding the wet product into 4.5L of water, fully stirring for 2 hours at 90 ℃, and then carrying out solid-liquid separation to obtain a filtrate A and a filter residue B; adding 100mL of 30% hydrogen peroxide into the filtrate A, introducing tail gas subjected to heat exchange, stirring for 1h at 40 ℃ after the reaction is finished, and performing solid-liquid separation to obtain a filtrate C containing ammonium chloride and a filter cake D containing aluminum-iron hydroxide, wherein the filtrate C is subjected to concentration and crystallization through hot gas subjected to heat exchange to obtain ammonium chloride which is used as an activating agent for recycling; fully mixing 25g of calcium aluminate with the filter cake D, adding 5% of industrial hydrochloric acid, adjusting the pH value to 2.2-2.5, stirring and reacting at 60-80 ℃ for 4 hours, and standing for 2 hours after the reaction is finished to obtain a solution E containing polyaluminum ferric chloride; crushing the filter residue B, transferring the crushed filter residue B into a corrosion-resistant high-pressure reaction kettle containing 6L of 25% sodium hydroxide solution, heating to 130 ℃, stirring for reaction for 4 hours, cooling to room temperature, and carrying out solid-liquid separation to obtain a solution F containing sodium silicate; according to the mass ratio of 1:1, slowly adding the solution E into the solution F, stirring at the speed of 180 r/min, reacting at the temperature of 40 ℃, adding 5% industrial hydrochloric acid after the solution C is added, adjusting the pH value to 3.5-4, and standing for 12h to obtain the yellowish-brown polymeric aluminum ferric silicate flocculant.
Example 2
Taking 1000g of the mixed raw material in the embodiment 1, ball-milling and crushing the mixed raw material to more than 100 meshes, and uniformly mixing the mixed raw material with an activating agent to prepare a raw material, wherein the activating agent is ammonium sulfate, and the mass ratio of the activating agent to the mixed raw material is 8: 1; transferring the prepared raw material into a roasting furnace to roast at 650 ℃, wherein the reaction pressure is 0.3MPa, and obtaining clinker and tail gas after roasting for 2 hours; cooling the tail gas through two stages of heat exchange procedures, wherein medium-high temperature hot gas at 300-350 ℃ is obtained after the first stage procedure, medium-temperature hot gas at 100-150 ℃ is obtained after the second stage procedure, and the medium-high temperature hot gas and the medium-temperature hot gas are used for the subsequent concentration and crystallization step of the solution; transferring the clinker into 1.5L of water for water quenching to obtain a crude product with the particle size of 10-100 mu m, wet-grinding the crude product, adding the wet product into 4.5L of water, fully stirring for 2 hours at 90 ℃, and then carrying out solid-liquid separation to obtain a filtrate A and a filter residue B; adding 100mL of 30% hydrogen peroxide into the filtrate A, introducing tail gas subjected to heat exchange, stirring for 1h at 40 ℃ after the reaction is finished, and performing solid-liquid separation to obtain a filtrate C containing ammonium sulfate and a filter cake D containing aluminum-iron hydroxide, wherein the filtrate C is subjected to concentration and crystallization through hot gas subjected to heat exchange to obtain ammonium sulfate which is used as an activating agent for recycling; fully mixing 25g of calcium aluminate with the filter cake D, adding 10% industrial sulfuric acid, adjusting the pH value to 2.2-2.5, stirring and reacting at 60-80 ℃ for 4 hours, and standing for 2 hours after the reaction is finished to obtain a solution E containing polymeric aluminum ferric sulfate; crushing the filter residue B, transferring the crushed filter residue B into a corrosion-resistant high-pressure reaction kettle containing 6L of 25% sodium hydroxide solution, heating to 130 ℃, stirring for reaction for 4 hours, cooling to room temperature, and carrying out solid-liquid separation to obtain a solution F containing sodium silicate; according to the mass ratio of 1:1, slowly adding the solution E into the solution F, stirring at 180 revolutions per minute at the reaction temperature of 40 ℃, adding 10 percent industrial sulfuric acid to adjust the pH value to 3.5-4 after the solution C is added, and standing for 12 hours to obtain the yellowish-brown polymeric aluminum ferric silicate flocculant.
Example 3
Mixing 5% industrial hydrochloric acid and 10% industrial sulfuric acid in a ratio of 1:1 to obtain inorganic acid; taking 1000g of the mixed raw material in the embodiment 1, ball-milling and crushing the mixed raw material to more than 100 meshes, and uniformly mixing the mixed raw material with an activating agent to prepare a raw material, wherein the activating agent is a mixture of ammonium chloride and ammonium sulfate in a mass ratio of 1:1, and the mass ratio of the activating agent to the mixed raw material is 8: 1; transferring the prepared raw material to a roasting furnace to roast at 650 ℃, wherein the reaction pressure is 0.3MPa, and roasting is carried out for 2h to obtain clinker and tail gas; cooling the tail gas through two stages of heat exchange procedures, wherein medium-high temperature hot gas at 300-350 ℃ is obtained after the first stage procedure, medium-temperature hot gas at 100-150 ℃ is obtained after the second stage procedure, and the medium-high temperature hot gas and the medium-temperature hot gas are used for the subsequent concentration and crystallization step of the solution; transferring the clinker into 1.5L of water for water quenching to obtain a crude product with the particle size of 10-100 mu m, wet-grinding the crude product, adding the wet product into 4.5L of water, fully stirring for 2 hours at 90 ℃, and then carrying out solid-liquid separation to obtain a filtrate A and a filter residue B; adding 100mL of 30% hydrogen peroxide into the filtrate A, introducing tail gas subjected to heat exchange, stirring for 1h at 40 ℃ after the reaction is finished, and performing solid-liquid separation to obtain a filtrate C containing ammonium chloride and ammonium sulfate and a filter cake D containing aluminum-iron hydroxide, wherein the filtrate C is subjected to concentration and crystallization through hot gas subjected to heat exchange to obtain ammonium chloride and ammonium sulfate which are used as activating agents for recycling; fully mixing 25g of calcium aluminate with the filter cake D, adding inorganic acid, adjusting the pH value to 2.2-2.5, stirring and reacting for 4 hours at the temperature of 60-80 ℃, and standing for 2 hours after the reaction is finished to obtain a solution E; crushing the filter residue B, transferring the crushed filter residue B into a corrosion-resistant high-pressure reaction kettle containing 6L of 25% sodium hydroxide solution, heating to 130 ℃, stirring for reaction for 4 hours, cooling to room temperature, and carrying out solid-liquid separation to obtain a solution F containing sodium silicate; according to the mass ratio of 1:1, slowly adding the solution E into the solution F, stirring at the speed of 180 r/min, reacting at the temperature of 40 ℃, adding an inorganic acid after the solution C is added, adjusting the pH value to 3.5-4, and standing for 12 hours to obtain the yellowish-brown polymeric aluminum ferric silicate flocculant.
Claims (6)
1. A preparation method of a polymeric aluminum ferric silicate flocculant is characterized by comprising the following steps: the method for preparing the polyaluminum ferric silicate flocculant by using one or more of coal gangue, fly ash and red mud as raw materials comprises the following steps:
(1) one or more of coal gangue, fly ash and red mud is crushed to more than 100 meshes by a ball mill to be used as a mixed raw material, wherein the ratio of Si/Al/Fe in the mixed raw material is 5-30/20-50/10-40;
(2) uniformly mixing the mixed raw material in the step (1) with an activating agent to prepare a raw material, wherein the activating agent is ammonium sulfate or ammonium chloride or a mixture of the ammonium sulfate and the ammonium chloride, and the mass ratio of the activating agent to the mixed raw material is (5-10): 1;
(3) roasting the raw material in the step (2) at 500-750 ℃ for 1-3 h, wherein the reaction pressure is 0.25-0.3 MPa, so as to obtain clinker and tail gas, carrying out heat exchange on the tail gas, and then, carrying out the next process step, wherein hot gas obtained after the heat exchange is used for the next concentration and crystallization step of the solution;
(4) transferring the clinker in the step (3) into water with the same mass for water quenching to obtain a crude product with the particle size of 10-100 microns, wet-grinding the crude product, adding water with the volume of 3 times that of the crude product, fully stirring for 2 hours at 90 ℃, and then carrying out solid-liquid separation to obtain a filtrate A and a filter residue B;
(5) adding hydrogen peroxide with the concentration of 30% into the filtrate A, then introducing tail gas subjected to heat exchange in the step (3), stirring for 1h at 40 ℃ after the reaction is finished, and performing solid-liquid separation to obtain a filtrate C and a filter cake D, wherein the filtrate C is used as an activating agent in the step (2) for recycling after being concentrated and crystallized;
(6) fully mixing calcium aluminate with the filter cake D, adding inorganic acid, stirring and reacting for 4 hours at the temperature of 60-80 ℃, and standing for 2 hours after the reaction is finished to obtain a solution E;
(7) crushing the filter residue B, transferring the crushed filter residue B into a corrosion-resistant high-pressure reaction kettle filled with a sodium hydroxide solution, heating to 130 ℃, stirring for reaction for 4 hours, cooling to room temperature, and carrying out solid-liquid separation to obtain a solution F;
(8) mixing the solution E with a solvent according to the mass ratio of (1-1.5): 1 is slowly added into the solution F at a stirring speed of not less than 150 revolutions per minute and a reaction temperature of 40 ℃, the solution C is added, inorganic acid is added to adjust the pH value to 3.5-4, and the solution C is kept stand for 6-12 hours to obtain a polymeric aluminum ferric silicate flocculant;
and (3) carrying out two-stage heat exchange on the tail gas in the step (3), obtaining medium-high temperature hot gas at 300-350 ℃ after the first stage, obtaining medium-temperature hot gas at 100-150 ℃ after the second stage, and using the medium-high temperature hot gas and the medium-temperature hot gas in the concentration and crystallization process of the filtrate C in the step (5).
2. The method for preparing polymeric aluminum ferric silicate flocculant according to claim 1, wherein the method comprises the following steps: in the step (6), the calcium aluminate accounts for 2-5% of the mass of the filter cake D, and after the inorganic acid is added, the pH value is adjusted to 2.2-2.5.
3. The method for preparing polymeric aluminum ferric silicate flocculant according to claim 1, wherein the method comprises the following steps: and (5) adding inorganic acid in the step (6) and adjusting the pH value to 2.2-2.5.
4. The method for preparing polymeric aluminum ferric silicate flocculant according to claim 1, wherein the method comprises the following steps: the inorganic acid in the step (6) and the step (8) is 3-10% of industrial hydrochloric acid or 5-15% of industrial sulfuric acid or a mixture of the two.
5. According to claimThe preparation method of the polymeric aluminum ferric silicate flocculant of claim 1 is characterized by comprising the following steps: na in the sodium hydroxide solution in the step (7)2O and SiO in filter residue B2The mass ratio of (A) to (B) is controlled to be 1 (0.6-0.8).
6. A polymeric aluminum ferric silicate flocculant is characterized in that: produced using the method of any one of claims 1-5.
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