CN111514748A - Wide-temperature flue gas dry desulfurizing agent for moving bed process and preparation method thereof - Google Patents
Wide-temperature flue gas dry desulfurizing agent for moving bed process and preparation method thereof Download PDFInfo
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Abstract
The invention provides a wide-temperature flue gas dry desulfurizing agent for a moving bed process, which is prepared from the following raw materials in parts by weight: 60-90 parts of active component, 0.2-1 part of metal oxide and 10-40 parts of carrier. According to the preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, when the active component calcium hydroxide is prepared, the roasted limestone ore raw material is adopted, and the potassium hydroxide solution is used for digestion, so that the porosity of the active component is increased, the electronic characteristic of the active component calcium is modulated through full contact of a potassium electronic auxiliary agent and the active component calcium, the sulfur dioxide adsorption performance of the active component calcium is improved, and the high-activity raw material is prepared. The flue gas desulfurizer of the invention has radial strength of more than or equal to 100N/cm and high strength, and can not cause secondary dust exceeding when being used for moving bed process desulfurization. The flue gas desulfurizer of the invention has the characteristics of high desulfurization efficiency, high sulfur capacity and wide use temperature (40-400 ℃).
Description
Technical Field
The invention belongs to the technical field of flue gas desulfurization and purification, and particularly relates to a wide-temperature flue gas dry desulfurizing agent for a moving bed process and a preparation method thereof.
Background
With the transformation of the electric power industry over, the non-electric power industry becomes the next reductionSO2Control point of discharge. But because of the characteristics of flue gas and the temperature characteristics of a boiler, the inherent technical defects of the traditional wet method and the semi-dry method cause the defects of large temperature drop, large pollution and the like, and the moving bed dry method is used as a new technology and has the characteristics of low flue gas desulfurization temperature (less than 10 ℃), no equipment corrosion, no sewage and waste acid generation, less secondary pollution, no scaling, high blockage reliability, low investment cost, small occupied area and the like, and in addition, the characteristics of integrating desulfurization and dust removal are integrated.
SO with new environmental policy2The emission requirements are more strict, and the method has a great deal of requirements in the smoke emission industries such as industrial boilers, glass ceramic furnaces, cement furnaces, ferrous metallurgy sintering furnaces, garbage incinerators, coking and petrochemical system cracking equipment and the like. The flue gas temperature range of the industries is wide, the treatment technology is difficult, and no desulfurizer product applicable to wide-temperature dry desulphurization exists in the current market.
Therefore, the development of the dry flue gas desulfurizer with a wide application temperature range, which is matched with a moving bed process for flue gas dry desulfurization, can solve a great technical problem for enterprises.
Disclosure of Invention
In view of the above, the invention aims to provide a wide-temperature flue gas dry desulfurizing agent for a moving bed process and a preparation method thereof, wherein a self-made strong active component is adopted, a small amount of metal oxide is added to obtain a high-activity desulfurizing agent, the strength and porosity of the desulfurizing agent are greatly improved by adopting ammonia steam curing and vacuum forming methods, and the problems of secondary dust exceeding and waste treatment when the desulfurizing agent is applied to the moving bed process are avoided.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight:
60-90 parts of active components, namely,
0.2 to 1 part of metal oxide,
10-40 parts of a carrier;
the active component is a mixture of calcium hydroxide and potassium hydroxide; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide.
Preferably, the wide-temperature flue gas dry desulfurizing agent for the moving bed process is prepared from the following raw materials in parts by weight:
60-80 parts of active components, namely,
0.2 to 0.6 portion of metal oxide,
10-30 parts of a carrier;
the active component is a mixture of calcium hydroxide and potassium hydroxide; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide.
Further, the mass ratio of potassium hydroxide to calcium hydroxide in the active component is 1: 50-200.
Further, the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10-20: 1-2.
Further, the carrier is at least one of gypsum or fly ash; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 0.5-2.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving the potassium hydroxide in water to obtain a digestion solution, wherein the mass concentration of total salts in the digestion solution is 0.5-5%;
(2) digesting the roasted limestone ore for 6-24h by the digestion solution to obtain a strong active component raw material;
(3) dissolving the metal oxide in acid to obtain impregnation liquid;
(4) mixing the raw materials with the strong active components with a carrier for 10-60min, adding the mixed powder into the impregnation liquid, and continuously mixing for 10-60min to obtain a wet material;
(5) feeding the wet material into a vacuum extruder, and performing extrusion molding to obtain a wet material;
(6) maintaining the wet material for 10-60min under the condition of ammonia steam;
(7) and drying the cured materials to obtain the wide-temperature flue gas dry desulfurizing agent for the moving bed process.
The finished radial strength of the wide-temperature flue gas dry desulfurizing agent for the moving bed process is more than or equal to 100N/cm.
Further, the acid in the step (3) is one of nitric acid, hydrochloric acid or sulfuric acid; the total salt mass concentration of the steeping liquor in the step (3) is 5-15%.
Further, the mass ratio of ammonia to water in the ammonia vapor in the step (6) is 1: 100-500.
Further, the drying temperature in the step (7) is 60-300 ℃, and the drying time is 0.5-6 h.
The wide-temperature flue gas dry desulfurizing agent for the moving bed process is applied to a moving bed reactor.
Further, the operation conditions of flue gas desulfurization of the moving bed reactor are as follows: 40-400 ℃ and gas space velocity of 100--1And the sulfur concentration is 35-5000mg/Nm3Inlet dust is less than or equal to 100mg/Nm3And the smoke outlet meets the following requirements: sulfur concentration is less than or equal to 30mg/Nm3The outlet dust is less than or equal to 10mg/Nm3And unit consumption of a desulfurizing agent: the amount of the 1kg of sulfur dioxide consumed the desulfurization agent is less than or equal to 3 kg.
Compared with the prior art, the wide-temperature flue gas dry desulfurizing agent for the moving bed process and the preparation method thereof have the following advantages:
(1) according to the preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, when the active component calcium hydroxide is prepared, the roasted limestone ore raw material is adopted, and the potassium hydroxide solution is used for digestion, so that the porosity of the active component is increased, the electronic characteristic of the active component calcium is modulated through full contact of a potassium electronic auxiliary agent and the active component calcium, the sulfur dioxide adsorption performance of the active component calcium is improved, and the high-activity raw material is prepared; the potassium hydroxide has high activity at different reaction temperatures due to digestion, and can quickly adsorb and absorb SO2The desulfurization efficiency at different temperatures is enhanced, and the effect of wide temperature is achieved.
(2) The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process adopts a potassium hydroxide digestion method, an ammonia-containing steam curing method and a vacuum method, the prepared desulfurizing agent has the characteristics of high strength, high desulfurizing efficiency, high sulfur capacity, wide use temperature range (40-400 ℃) and the like, and the key points are that the desulfurizing product is calcium sulfate and calcium sulfite is avoided, so that the desulfurizing product can be recycled, and the problems of secondary pollution to enterprises or difficult disposal of the desulfurizing product and the like are avoided.
(3) The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process further activates the wide-temperature flue gas dry desulfurizing agent for the moving bed process through the curing treatment of ammonia-containing steam, and the ammonia steam provides an alkaline environment, so that the specific surface area of the desulfurizing agent is favorably formed, and the surface activity of an active component calcium hydroxide of the desulfurizing agent is excited. The quick sulfur absorption and low-temperature desulfurization performance of the sulfur absorbent are enhanced.
(4) The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, disclosed by the invention, has the advantages that the porosity of the desulfurizing agent is not reduced when the performance of the desulfurizing agent is improved by a vacuum forming means and a subsequent ammonia-containing steam curing means, so that the prepared desulfurizing agent has high strength, high desulfurizing efficiency and high sulfur capacity, and is suitable for the requirement of a moving bed on the high strength of the desulfurizing agent.
(5) The wide-temperature flue gas dry desulfurizing agent for the moving bed process is modified by three substances of metal oxides of titanium oxide, strontium oxide and zirconium oxide, the adsorption-absorption-conversion performance of sulfur dioxide is enhanced, metal salt reacts with the surface of calcium hydroxide small particles, while part of calcium sulfate is generated, metal hydroxide precipitate is generated around the calcium sulfate, thereby preventing agglomeration among calcium sulfate particles from blocking surface pore channels of the calcium hydroxide, thereby, when the desulfurizer is subsequently applied, the sulfur dioxide is easier to transfer mass and enter the calcium hydroxide particles for reaction, the calcium utilization rate of the desulfurizer is increased, the prepared wide-temperature flue gas dry desulfurizer has good desulfurization effect at the application temperature of 40-400 ℃, the metal oxide can play a role in enriching oxygen and catalyzing in the reaction process, simultaneously enhances the wear-resisting property of the desulfurizer, and reduces the dust amount generated by the friction between the desulfurizer and the bed body in the moving process.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 75 parts of active component, 0.24 part of metal oxide and 24.76 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide, and the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10: 1; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 1.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 11.1g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 2.2%;
(2) weighing 1350.13g limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4h, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6h-24h, and obtaining the raw material with strong active components;
(3) weighing 3g of titanium oxide, 0.3g of strontium oxide and 0.3g of zirconium oxide, dissolving in 50mL of 5% nitric acid solution by mass concentration, stirring, heating and dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 185.7g of fly ash and 185.7g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing ammonia water with the mass ratio of ammonia to water of 1:200 into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, wherein an activating gas is ammonia vapor, heating to 200 ℃ within 10min, activating for 30min, rotating at a speed of 5r/h and a lifting angle of 5 ℃, and cooling and taking out;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Example 2
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 75 parts of active component, 0.24 part of metal oxide and 24.76 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:200 of a carrier; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide, and the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10: 1; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 1.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 5.6g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 1.1%;
(2) weighing 1356.85g limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4h, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6h-24h, and obtaining the raw material with strong active components;
(3) weighing 3g of titanium oxide, 0.3g of strontium oxide and 0.3g of zirconium oxide, dissolving in 50mL of 5% nitric acid solution by mass concentration, stirring, heating and dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 185.7g of fly ash and 185.7g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing prepared ammonia water into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, heating to 200 ℃ within 10min by using activating gas, activating for 30min at the rotating speed of 5r/h and the lifting angle of 5 ℃, and cooling and taking out the wet material;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Example 3
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 75 parts of active component, 0.575 parts of metal oxide and 24.425 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide, and the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:20: 2; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 1.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 11.1g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 2.2%;
(2) weighing 1350.1g of limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4 hours, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6-24 hours, and obtaining the raw material with strong active components;
(3) weighing 7.5g of titanium oxide, 0.375g of strontium oxide and 0.75g of zirconium oxide, dissolving in 50mL of 5% nitric acid solution by mass concentration, stirring, heating, dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 183.1875g of fly ash and 183.1875g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing prepared ammonia water into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, heating to 200 ℃ within 10min by using activating gas, activating for 30min at the rotating speed of 5r/h and the lifting angle of 5 ℃, and cooling and taking out the wet material;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Example 4
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 65 parts of active component, 0.24 part of metal oxide and 34.76 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide, and the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10: 1; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 2.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 9.65g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 1.89%;
(2) weighing 1170.1g of limestone ore sample, crushing into blocks, heating, roasting and heating to 895-1050 ℃, continuously roasting for 4h, taking out and cooling after gas is exhausted, primarily crushing the roasted and cooled limestone ore, then putting the prepared digestion solution into a beaker for digestion for 6h-24h, and obtaining the strong active component raw material;
(3) weighing 3g of titanium oxide, 0.3g of strontium oxide and 0.3g of zirconium oxide, dissolving in 50mL of 5% nitric acid solution by mass concentration, stirring, heating and dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 347.6g of fly ash and 173.8g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing ammonia water with the mass ratio of ammonia to water of 1:200 into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, wherein an activating gas is ammonia vapor, heating to 200 ℃ within 10min, activating for 30min, rotating at a speed of 5r/h and a lifting angle of 5 ℃, and cooling and taking out;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Example 5
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 65 parts of active component, 0.24 part of metal oxide and 34.76 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide, and the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10: 1; the carrier is fly ash.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 9.65g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 1.89%;
(2) weighing 1170.12g limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4h, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6h-24h, and obtaining the raw material with strong active components;
(3) weighing 3g of titanium oxide, 0.3g of strontium oxide and 0.3g of zirconium oxide, dissolving in 50mL of 5% nitric acid solution by mass concentration, stirring, heating and dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 521.4g of fly ash, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, then adding the impregnation liquid prepared in the step (3), and then resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing ammonia water with the mass ratio of ammonia to water of 1:200 into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, wherein an activating gas is ammonia vapor, heating to 200 ℃ within 10min, activating for 30min, rotating at a speed of 5r/h and a lifting angle of 5 ℃, and cooling and taking out;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Example 6
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 65 parts of active component, 0.24 part of metal oxide and 34.76 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide, and the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10: 1; the carrier is gypsum.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 9.65g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 1.89%;
(2) weighing 1170.1g of limestone ore sample, crushing into blocks, heating, roasting and heating to 895-1050 ℃, continuously roasting for 4h, taking out and cooling after gas is exhausted, primarily crushing the roasted and cooled limestone ore, then putting the prepared digestion solution into a beaker for digestion for 6h-24h, and obtaining the strong active component raw material;
(3) weighing 3g of titanium oxide, 0.3g of strontium oxide and 0.3g of zirconium oxide, dissolving in 50mL of 5% nitric acid solution by mass concentration, stirring, heating and dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 521.4g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, then adding the impregnation liquid prepared in the step (3), and then resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing ammonia water with the mass ratio of ammonia to water of 1:200 into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, wherein an activating gas is ammonia vapor, heating to 200 ℃ within 10min, activating for 30min, rotating at a speed of 5r/h and a lifting angle of 5 ℃, and cooling and taking out;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Comparative example 1
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 75 parts of active component, 0.575 parts of metal oxide and 24.425 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is titanium oxide; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 1.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 11.1g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 2.2%;
(2) weighing 1350.1g of limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4 hours, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6-24 hours, and obtaining the raw material with strong active components;
(3) weighing 8.625g of titanium oxide, dissolving the titanium oxide in 50mL of nitric acid solution with the mass concentration of 5%, stirring, heating, dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 183.1875g of fly ash and 183.1875g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing prepared ammonia water into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, heating to 200 ℃ within 10min by using activating gas, activating for 30min at the rotating speed of 5r/h and the lifting angle of 5 ℃, and cooling and taking out the wet material;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Comparative example 2
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 75 parts of active component, 0.575 parts of metal oxide and 24.425 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is strontium oxide; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 1.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 11.1g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 2.2%;
(2) weighing 1350.1g of limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4 hours, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6-24 hours, and obtaining the raw material with strong active components;
(3) weighing 8.625g of strontium oxide, dissolving the strontium oxide in 50mL of 5% nitric acid solution by mass concentration, stirring, heating and dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 183.1875g of fly ash and 183.1875g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing prepared ammonia water into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, heating to 200 ℃ within 10min by using activating gas, activating for 30min at the rotating speed of 5r/h and the lifting angle of 5 ℃, and cooling and taking out the wet material;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Comparative example 3
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 75 parts of active component, 0.575 parts of metal oxide and 24.425 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is zirconium oxide; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 1.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 11.1g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 2.2%;
(2) weighing 1350.1g of limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4 hours, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6-24 hours, and obtaining the raw material with strong active components;
(3) weighing 8.625g of zirconia, dissolving in 50mL of nitric acid solution with the mass concentration of 5%, stirring, heating, dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 183.1875g of fly ash and 183.1875g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) introducing prepared ammonia water into a water filling port of an atmosphere rotary furnace in the atmosphere rotary furnace, heating to 200 ℃ within 10min by using activating gas, activating for 30min at the rotating speed of 5r/h and the lifting angle of 5 ℃, and cooling and taking out the wet material;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
Comparative example 4
A wide-temperature flue gas dry desulfurizing agent for a moving bed process is prepared from the following raw materials in parts by weight: 75 parts of active component, 0.24 part of metal oxide and 24.76 parts of carrier; the active component is a mixture of calcium hydroxide and potassium hydroxide, and the mass ratio of the potassium hydroxide to the calcium hydroxide in the active component is 1:100, respectively; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide, and the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10: 1; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 1.
The preparation method of the wide-temperature flue gas dry desulfurizing agent for the moving bed process comprises the following steps:
(1) dissolving 11.1g of potassium hydroxide in 500mL of water to obtain a digestion solution with the mass concentration of 2.2%;
(2) weighing 1350.1g of limestone ore samples, crushing the limestone ore samples into blocks, heating, roasting and heating to the temperature of 895-1050 ℃, continuously roasting for 4 hours, taking out the limestone ore samples after gas is exhausted, cooling, preliminarily crushing the roasted and cooled limestone ore, putting the prepared digestion solution into a beaker for digestion for 6-24 hours, and obtaining the raw material with strong active components;
(3) weighing 3g of titanium oxide, 0.3g of strontium oxide and 0.3g of zirconium oxide, dissolving in 50mL of 5% nitric acid solution by mass concentration, stirring, heating and dissolving uniformly, and standing for 10min to obtain a steeping fluid;
(4) weighing 185.7g of fly ash and 185.7g of gypsum, crushing, putting the crushed powder and the strong active component raw material into a mechanical stirrer, mixing for 30min, adding the impregnation liquid prepared in the step (3), and resetting the mixing time of the mechanical stirrer to be 30min to obtain a wet material;
(5) putting the wet material into a vacuum extruder for extrusion molding to obtain a strip-shaped wet finished product with the particle size of 6mm, standing for 1h, and then solidifying and molding to obtain the wet material;
(6) heating the extruded wet material in an atmosphere rotary furnace, wherein the activating gas is water vapor, heating to 200 ℃ within 10min under the condition of containing the steam, activating for 30min, rotating at the speed of 5r/h and at the lifting angle of 5 ℃, and cooling and taking out;
(7) and drying the cured and activated material at the drying temperature of 300 ℃ for 3h to obtain the finished product of the wide-temperature flue gas dry desulfurizing agent for the moving bed process, wherein the radial strength of the finished product is more than or equal to 100N/cm.
The performance of the wide temperature flue gas dry desulfurization agent finished products for the moving bed process obtained in examples 1-6 and comparative examples 1-4 was tested by using a chemical analyzer and a desulfurization evaluation mechanism, and the physicochemical properties of the finished reactants prepared by the above method are shown in table 1.
TABLE 1 physicochemical Properties
The desulfurization efficiency test is carried out on the sample in the example 1, the flow rate of the simulated flue gas is 0.25m/s, and the space velocity of the desulfurizing agent is 100--1. Inlet flue gas SO2The concentration is 35-5000mg/Nm3Inlet dust is less than or equal to 100mg/Nm3The concentration of nitrogen oxide is 400mg/m3The water content is 12.1%, 3 temperature values are selected for the flue gas temperature in the range of 40-400 ℃, and the flue gas desulfurization and purification efficiency index is shown in table 2.
TABLE 2 flue gas desulfurization purification efficiency
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A wide temperature flue gas dry desulfurizing agent for moving bed process is characterized in that: the feed is prepared from the following raw materials in parts by weight:
60-90 parts of active components, namely,
0.2 to 1 part of metal oxide,
10-40 parts of a carrier;
the active component is a mixture of calcium hydroxide and potassium hydroxide; the metal oxide is a mixture of strontium oxide, titanium oxide and zirconium oxide.
2. The wide-temperature flue gas dry desulfurization agent for a moving bed process according to claim 1, characterized in that: the mass ratio of potassium hydroxide to calcium hydroxide in the active components is 1: 50-200.
3. The wide-temperature flue gas dry desulfurization agent for a moving bed process according to claim 1, characterized in that: the mass ratio of the strontium oxide to the titanium oxide to the zirconium oxide is 1:10-20: 1-2.
4. The wide-temperature flue gas dry desulfurization agent for a moving bed process according to claim 1, characterized in that: the carrier is at least one of gypsum or fly ash; the carrier is a mixture of gypsum and fly ash, and the mass ratio of the gypsum to the fly ash is 1: 0.5-2.
5. The method for preparing a wide-temperature flue gas dry desulfurizing agent for a moving bed process according to any one of claims 1 to 4, wherein the method comprises the following steps: the method comprises the following steps:
(1) dissolving the potassium hydroxide in water to obtain a digestion solution, wherein the mass concentration of total salts in the digestion solution is 0.5-5%;
(2) digesting the roasted limestone ore for 6-24h by the digestion solution to obtain a strong active component raw material;
(3) dissolving the metal oxide in acid to obtain impregnation liquid;
(4) mixing the raw materials with the strong active components with a carrier for 10-60min, adding the mixed powder into the impregnation liquid, and continuously mixing for 10-60min to obtain a wet material;
(5) feeding the wet material into a vacuum extruder, and performing extrusion molding to obtain a wet material;
(6) maintaining the wet material for 10-60min under the condition of ammonia steam;
(7) and drying the cured materials to obtain the wide-temperature flue gas dry desulfurizing agent for the moving bed process.
6. The method for preparing the wide-temperature flue gas dry desulfurizing agent for the moving bed process according to claim 5, which is characterized in that: the acid in the step (3) is one of nitric acid, hydrochloric acid or sulfuric acid; the total salt mass concentration of the steeping liquor in the step (3) is 5-15%.
7. The method for preparing the wide-temperature flue gas dry desulfurizing agent for the moving bed process according to claim 5, which is characterized in that: the mass ratio of ammonia to water in the ammonia vapor in the step (6) is 1: 100-500.
8. The method for preparing the wide-temperature flue gas dry desulfurizing agent for the moving bed process according to claim 5, which is characterized in that: the drying temperature in the step (7) is 60-300 ℃, and the drying time is 0.5-6 h.
9. Use of the wide temperature flue gas dry desulfurization agent for moving bed processes according to any one of claims 1 to 4, characterized in that: the wide-temperature flue gas dry desulfurizing agent for the moving bed process is applied to a moving bed reactor.
10. Use of a wide temperature flue gas dry desulfurization agent for a moving bed process according to claim 9, characterized in that: the operation conditions of the flue gas desulfurization of the moving bed reactor are as follows: 40-400 ℃ and gas space velocity of 100--1And the sulfur concentration is 35-5000mg/Nm3Inlet dust is less than or equal to 100mg/Nm3And the smoke outlet meets the following requirements: sulfur concentration is less than or equal to 30mg/Nm3The outlet dust is less than or equal to 10mg/Nm3And unit consumption of a desulfurizing agent: the amount of the 1kg of sulfur dioxide consumed the desulfurization agent is less than or equal to 3 kg.
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