CN113578276A - Preparation method of wide-temperature selective adsorption replacement desulfurization material - Google Patents
Preparation method of wide-temperature selective adsorption replacement desulfurization material Download PDFInfo
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- B01D2257/708—Volatile organic compounds V.O.C.'s
Abstract
The invention discloses a preparation method of a wide-temperature selection type adsorption replacement desulfurization material, which comprises the steps of carrying out mixing reaction on potassium permanganate, methanol and manganese sulfate to prepare manganese oxide, then mixing the manganese oxide, transition metal oxide, polymeric aluminum oxide and an accelerant, dripping an emulsifier at a constant speed through a burette during stirring to prepare desulfurization emulsion, placing the prepared desulfurization emulsion in a vacuum low-temperature dryer to prepare a desulfurization base material, finally placing the prepared desulfurization base material in a shaping mold, then the shaping mould is placed in a formation box for formation to prepare the adsorption displacement desulfurization material, the novel nano catalytic adsorption material which takes manganese oxide as a main raw material can be used for desulfurization in a wide temperature window, and has high adsorption capacity and adsorption rate, and the saturated material can be recycled by a simpler method.
Description
Technical Field
The invention relates to the technical field of desulfurization, in particular to a preparation method of a wide-temperature selective adsorption replacement desulfurization material.
Background
The rapid development of industrialization has promoted the rapid development of scientific and technological progress in society, but human beings have suffered from various environmental pollution problems caused by fossil fuels and the like while enjoying scientific and technological achievements. The emission of sulfur oxides and nitrogen oxides is a main source of air pollution, is a main substance forming acid rain, and has serious influence on the survival and life of human beings.
Disclosure of Invention
The invention aims to provide a preparation method of a wide-temperature selective adsorption replacement desulfurization material, which solves the following technical problems:
the desulfurization material has a small temperature range in use, and is liable to generate a high exothermic or endothermic reaction, increasing the manufacturing cost of the desulfurization equipment.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a wide-temperature selective adsorption displacement desulfurization material comprises the following steps:
step A1: mixing potassium permanganate, methanol and manganese sulfate for reaction, controlling the temperature to be 25-40 ℃ until the reaction is complete to prepare manganese oxide, and adjusting the pH value to be neutral;
step A2: mixing manganese oxide, transition metal oxide, polymeric aluminum oxide and an accelerant, keeping the temperature at 40-45 ℃, stirring for 10-15min at the rotating speed of 50-150r/min, dropwise adding an emulsifier at a constant speed through a burette during stirring, and standing for 2-3 h to prepare a desulfurization emulsion;
step A3: placing the prepared desulfurization emulsion in a vacuum low-temperature dryer, keeping the temperature between 100 ℃ below zero and 300 ℃ below zero, drying for 5 to 6 hours, and controlling the water content to be 2 to 2.5 percent to prepare a desulfurization base material;
step A4: and placing the prepared desulfurization base material into a shaping mold, and then placing the shaping mold into a forming box for forming to prepare the adsorption displacement desulfurization material.
As a further scheme of the invention: the emulsifier is prepared by the following steps:
step S1: mixing and stirring photocatalyst titanium dioxide, acidified bentonite, lauric acid monoglyceride and alcohol, controlling the temperature of the solution to be 25-35 ℃, the stirring speed to be 100-120r/min and the stirring time to be 20-25min to prepare an emulsified base material;
step S2: adding deionized water into the obtained emulsified base material, maintaining at 20-25 deg.C, performing ultrasonic treatment at 40-50kHz for 40-45min to obtain emulsified solution, and adjusting pH to neutral;
step S3: and (3) putting the emulsified solution into an emulsifying box for emulsification, wherein the emulsifying temperature is 75-85 ℃, and standing for 1-1.5h to prepare the emulsifier.
As a further scheme of the invention: the dosage ratio of potassium permanganate, methanol and manganese sulfate in the step A1 is 10 g: 3.5-4.3mL, 5.3-6.7 g.
As a further scheme of the invention: the dosage ratio of the manganese oxide, the transition metal oxide, the polymeric aluminum oxide, the accelerator and the emulsifier in the step A2 is 10 mL: 3.5-4.2 g: 1.2-1.5 g: 0.5-0.7 mL: 0.4-0.8 g.
As a further scheme of the invention: the dosage ratio of the photocatalyst titanium dioxide, the acidified bentonite, the lauric acid monoglyceride and the alcohol in the step S1 is 10 g: 2.3-2.8 g: 1.5-1.7 g: 40-45mL, wherein the alcohol is reagent grade alcohol, and the alcohol concentration is 95%.
As a further scheme of the invention: the dosage ratio of the emulsified base material to the deionized water is 1 mL: 3.5-4 mL.
As a further scheme of the invention: in the step A1 and the step S2, sodium hydroxide solution is adopted for adjusting the pH, and the mass fraction of the sodium hydroxide solution is 12-15%.
As a further scheme of the invention: the transition metal oxide is one of calcium oxide, sodium oxide, iron oxide and copper oxide.
As a further scheme of the invention: the acidified bentonite is one of sodium-based acidified bentonite and calcium-based acidified bentonite.
As a further scheme of the invention: the accelerant is one of 3-methylthiazolidine-thione-2 and 1- (N-oxydiethylene thiocarbamoyl) -2- (N-oxydiethylene) thiobenzimidazole.
The invention has the beneficial effects that:
(1) according to the invention, the adsorption displacement desulfurization material is prepared from potassium permanganate, methanol, manganese sulfate, transition metal oxide, polymeric aluminum oxide and an accelerant, the desulfurization rate is high, the purification of formaldehyde, sulfur oxides, oxynitride and VOCs can be realized in two ways of active adsorption and passive adsorption, and in the desulfurization process, the heat release and heat absorption processes can not occur, the reaction condition requirement is reduced, the reaction equipment is simplified, the extrusion resistance is strong, the plasticity is high, the reaction rate is high, the adsorption displacement desulfurization material can adapt to large-air-volume desulfurization, and the use at the highest temperature of 500 ℃ can be met;
(2) in the invention, an emulsifier is added in the raw materials for preparing the adsorption replacement desulfurization material, and the emulsifier is prepared by reacting and processing raw materials such as photocatalyst titanium dioxide, acidified bentonite, lauric acid monoglyceride, alcohol and the like, wherein the combination of the photocatalyst silicon dioxide and the acidified bentonite plays a role in complementary improvement, the respective formaldehyde purification rate and purification rate are improved, and in the process of preparing the adsorption replacement desulfurization material, the emulsifier also improves the desulfurization reaction rate and effectively improves the formaldehyde removal rate at the same time of improving the surface tension of the material.
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The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention discloses the following two embodiments:
the first embodiment is as follows:
a preparation method of a wide-temperature selective adsorption displacement desulfurization material comprises the following steps:
step A1: mixing potassium permanganate, methanol and manganese sulfate according to the weight ratio of 10 g: 3.5mL of the manganese oxide is mixed and reacted with 5.3g of the sodium hydroxide solution according to the dosage ratio, the temperature is controlled to be 25 ℃ until the reaction is completed, the manganese oxide is prepared, and the pH value is adjusted to be neutral by using the sodium hydroxide solution with the mass fraction of 12%;
step A2: manganese oxide, transition metal oxide, polymeric alumina and accelerator were mixed in a 10 mL: 3.5 g: 1.2 g: 0.5 mL: 0.4g of the additive is mixed, the mixture is kept at 40 ℃, the mixture is stirred for 10min at the rotating speed of 50r/min, an emulsifier is dripped at a constant speed through a burette in the stirring process, then the mixture is kept stand for 2h to prepare a desulfurization emulsion, and an adsorption displacement desulfurization material is prepared from potassium permanganate, methanol and manganese sulfate, transition metal oxide, polymeric aluminum oxide and an accelerant.
Step A3: placing the prepared desulfurization emulsion in a vacuum low-temperature dryer, keeping the temperature at-100 ℃, drying for 5h, and controlling the water content to be 2% to prepare a desulfurization base material;
step A4: the prepared desulfurization base material is placed in a shaping mold, then the shaping mold is placed in a shaping box for formation, and an adsorption displacement desulfurization material is prepared, wherein the adsorption displacement desulfurization material uses a novel nano catalytic adsorption material with manganese oxide as a main raw material, can be desulfurized in a very wide temperature window, has very high adsorption capacity and adsorption rate, and most importantly, the saturated material can be recycled by a relatively simple method.
In the using process, the reaction principle of the adsorption displacement desulfurization material is that the surface of the adsorption displacement desulfurization material is provided with abundant catalytic active centers, SO that oxygen in the air can be converted into surface oxygen species with higher oxidation capacity, and the surface oxygen species can rapidly convert SO2The material is converted into surface sulfate radicals, secondly, a large number of alkaline adsorption active sites are arranged near the catalytic centers, the surface sulfate radicals can be fixed and stored in a large capacity, in addition, the use temperature can reach 500 ℃ at most when sulfur oxide compounds are removed, the adsorption priority of the sulfur oxide compounds can be ensured to be the highest, even if the material is adsorbed and saturated by other gases in advance, the sulfur oxide compounds can still be adsorbed, meanwhile, the previously adsorbed gases are released, and after the material is adsorbed and saturated, the sulfur oxide compounds are mainly captured and fixed in the form of surface manganese sulfate.
The emulsifier is prepared by the following steps:
step S1: mixing photocatalyst titanium dioxide, acidified bentonite, lauric acid monoglyceride and alcohol according to the weight ratio of 10 g: 2.3 g: 1.5 g: mixing and stirring 40mL of the mixture, controlling the temperature of the solution to be 25 ℃, the stirring speed to be 100r/min and the stirring time to be 20min, and preparing an emulsified base material, wherein the alcohol is reagent-grade alcohol and the alcohol concentration is 95%;
step S2: adding deionized water into the prepared emulsified base material, keeping the temperature at 20 ℃, carrying out ultrasonic treatment at 40kHz for 40min to prepare an emulsified solution, and adjusting the pH to be neutral by using a sodium hydroxide solution with the mass fraction of 12%, wherein the dosage ratio of the emulsified base material to the deionized water is 1 mL: 3.5 mL;
step S3: and (3) putting the emulsified solution into an emulsifying box for emulsification, wherein the emulsifying temperature is 75 ℃, and standing for 1h to prepare the emulsifier.
In the process of preparing the adsorption replacement desulfurization material, the emulsifier improves the desulfurization reaction rate and effectively improves the formaldehyde removal rate at the same time when improving the surface tension of the material, the formaldehyde degradation rate is 95 percent at the highest, and the carbon dioxide yield is 57 percent at the highest.
The transition metal oxide is one of calcium oxide, sodium oxide, iron oxide and copper oxide.
The acidified bentonite is one of sodium-based acidified bentonite and calcium-based acidified bentonite, the acidified bentonite has good filtering performance, and the acidified bentonite is added into the emulsifier, so that the circulation rate of air can be increased while desulfurization and formaldehyde removal are realized.
The accelerant is one of 3-methylthiazolidine-thione-2 and 1- (N-oxydiethylene thiocarbamoyl) -2- (N-oxydiethylene) thiobenzimidazole, and the accelerant has the function of anti-aging while being used as the accelerant to promote the reaction, thereby prolonging the service life of the adsorption replacement desulfurization material.
The application and technical selection of the adsorption displacement desulfurization material need to be selected according to specific use conditions: when the material meets industrial application, the adsorption replacement desulfurization material is not suitable for being made into granules, because the air speed is too high, the material can be discharged along with flue gas, so that the problems of material loss, loose tissue structure and the like can be caused, and the material is prepared into a honeycomb shape, so that the specific surface area of the material is not influenced, and the tissue architecture is complete and firm; when satisfying high standard and discharging, then need regularly change the material, in adsorbing replacement desulfurization process, the replacement process is big in the flue gas desulfurization device replacement degree of difficulty, consequently retrieves the replacement more feasible to also can reach cyclic utilization's purpose, reduce consumptive material and equipment cost.
Example two
A preparation method of a wide-temperature selective adsorption displacement desulfurization material comprises the following steps:
step A1: mixing potassium permanganate, methanol and manganese sulfate according to the weight ratio of 10 g: 4.3mL of the manganese oxide is mixed and reacted with 6.7g of the sodium hydroxide solution according to the dosage ratio, the temperature is controlled to be 40 ℃ until the reaction is completed, the manganese oxide is prepared, and the pH value is adjusted to be neutral by 15 percent of sodium hydroxide solution;
step A2: manganese oxide, transition metal oxide, polymeric alumina and accelerator were mixed in a 10 mL: 4.2 g: 1.5 g: 0.7 mL: 0.8g of the additive is mixed, the mixture is kept at 45 ℃, the mixture is stirred for 15min at the rotating speed of 150r/min, an emulsifier is dripped at a constant speed through a burette in the stirring process, then the mixture is kept stand for 3h to prepare a desulfurization emulsion, and an adsorption displacement desulfurization material is prepared from potassium permanganate, methanol and manganese sulfate, transition metal oxide, polymeric aluminum oxide and an accelerant.
Step A3: placing the prepared desulfurization emulsion in a vacuum low-temperature dryer, keeping the temperature at minus 300 ℃, drying for 6h, and controlling the water content to be 2.5% to prepare a desulfurization base material;
step A4: the prepared desulfurization base material is placed in a shaping mold, then the shaping mold is placed in a shaping box for formation, and an adsorption displacement desulfurization material is prepared, wherein the adsorption displacement desulfurization material uses a novel nano catalytic adsorption material with manganese oxide as a main raw material, can be desulfurized in a very wide temperature window, has very high adsorption capacity and adsorption rate, and most importantly, the saturated material can be recycled by a relatively simple method.
In the using process, the reaction principle of the adsorption displacement desulfurization material is that the surface of the adsorption displacement desulfurization material is provided with abundant catalytic active centers, SO that oxygen in the air can be converted into surface oxygen species with higher oxidation capacity, and the surface oxygen species can rapidly convert SO2Conversion to surface sulfates and, secondly, a large number of basic adsorption active sites in the vicinity of these catalytic centers, the possibility of fixing and storing these surface sulfates in large volumes and, in the removal of sulfur and oxygen compounds, the use temperatures up to 500 ℃ also ensure that the adsorption priority of sulfur and oxygen compounds is the highest, even if the material has previously been saturated by adsorption of other gasesThe material can still adsorb oxysulfide and release the gas adsorbed previously, and after the material is adsorbed and saturated, the oxysulfide is mainly captured and fixed in the form of surface manganese sulfate.
The emulsifier is prepared by the following steps:
step S1: mixing photocatalyst titanium dioxide, acidified bentonite, lauric acid monoglyceride and alcohol according to the weight ratio of 10 g: 2.8 g: 1.7 g: mixing and stirring 45mL of the mixture according to the dosage ratio, controlling the temperature of the solution to be 35 ℃, the stirring speed to be 120r/min and the stirring time to be 25min to prepare an emulsified base material, wherein the alcohol is reagent grade alcohol and the alcohol concentration is 95%;
step S2: adding deionized water into the prepared emulsified base material, keeping the temperature at 25 ℃, performing 50kHz ultrasonic treatment for 45min to prepare an emulsified solution, and adjusting the pH to be neutral by using a sodium hydroxide solution with the mass fraction of 15%, wherein the dosage ratio of the emulsified base material to the deionized water is 1 mL: 4 mL;
step S3: and (3) putting the emulsified solution into an emulsifying box for emulsification, wherein the emulsifying temperature is 85 ℃, and standing for 1.5 hours to obtain the emulsifier.
In the process of preparing the adsorption replacement desulfurization material, the emulsifier improves the desulfurization reaction rate and effectively improves the formaldehyde removal rate at the same time when improving the surface tension of the material, the formaldehyde degradation rate is 95 percent at the highest, and the carbon dioxide yield is 57 percent at the highest.
The transition metal oxide is one of calcium oxide, sodium oxide, iron oxide and copper oxide.
The acidified bentonite is one of sodium-based acidified bentonite and calcium-based acidified bentonite, the acidified bentonite has good filtering performance, and the acidified bentonite is added into the emulsifier, so that the circulation rate of air can be increased while desulfurization and formaldehyde removal are realized.
The accelerant is one of 3-methylthiazolidine-thione-2 and 1- (N-oxydiethylene thiocarbamoyl) -2- (N-oxydiethylene) thiobenzimidazole, and the accelerant has the function of anti-aging while being used as the accelerant to promote the reaction, thereby prolonging the service life of the adsorption replacement desulfurization material.
The application and technical selection of the adsorption displacement desulfurization material need to be selected according to specific use conditions: when the material meets industrial application, the adsorption replacement desulfurization material is not suitable for being made into granules, because the air speed is too high, the material can be discharged along with flue gas, so that the problems of material loss, loose tissue structure and the like can be caused, and the material is prepared into a honeycomb shape, so that the specific surface area of the material is not influenced, and the tissue architecture is complete and firm; when satisfying high standard and discharging, then need regularly change the material, in adsorbing replacement desulfurization process, the replacement process is big in the flue gas desulfurization device replacement degree of difficulty, consequently retrieves the replacement more feasible to also can reach cyclic utilization's purpose, reduce consumptive material and equipment cost.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. The preparation method of the wide-temperature selective adsorption displacement desulfurization material is characterized by comprising the following steps of:
step A1: mixing potassium permanganate, methanol and manganese sulfate for reaction, controlling the temperature to be 25-40 ℃ until the reaction is complete to prepare manganese oxide, and adjusting the pH value to be neutral;
step A2: mixing manganese oxide, transition metal oxide, polymeric aluminum oxide and an accelerant, keeping the temperature at 40-45 ℃, stirring for 10-15min at the rotating speed of 50-150r/min, dropwise adding an emulsifier at a constant speed through a burette during stirring, and standing for 2-3 h to prepare a desulfurization emulsion;
step A3: placing the prepared desulfurization emulsion in a vacuum low-temperature dryer, keeping the temperature between 100 ℃ below zero and 300 ℃ below zero, drying for 5 to 6 hours, and controlling the water content to be 2 to 2.5 percent to prepare a desulfurization base material;
step A4: and placing the prepared desulfurization base material into a shaping mold, and then placing the shaping mold into a forming box for forming to prepare the adsorption displacement desulfurization material.
2. The method for preparing the wide-temperature selective adsorption replacement desulfurization material according to claim 1, wherein the emulsifier is prepared by the following steps:
step S1: mixing and stirring photocatalyst titanium dioxide, acidified bentonite, lauric acid monoglyceride and alcohol, controlling the temperature of the solution to be 25-35 ℃, the stirring speed to be 100-120r/min and the stirring time to be 20-25min to prepare an emulsified base material;
step S2: adding deionized water into the obtained emulsified base material, maintaining at 20-25 deg.C, performing ultrasonic treatment at 40-50kHz for 40-45min to obtain emulsified solution, and adjusting pH to neutral;
step S3: and (3) putting the emulsified solution into an emulsifying box for emulsification, wherein the emulsifying temperature is 75-85 ℃, and standing for 1-1.5h to prepare the emulsifier.
3. The method for preparing the wide-temperature selective adsorption displacement desulfurization material according to claim 1, wherein the amount ratio of potassium permanganate, methanol and manganese sulfate in step A1 is 10 g: 3.5-4.3mL, 5.3-6.7 g.
4. The method for preparing the wide-temperature selective adsorption displacement desulfurization material according to claim 1, wherein the amount ratio of the manganese oxide, the transition metal oxide, the polymeric alumina, the promoter and the emulsifier in step A2 is 10 mL: 3.5-4.2 g: 1.2-1.5 g: 0.5-0.7 mL: 0.4-0.8 g.
5. The method for preparing the wide temperature selective adsorption replacement desulfurization material according to claim 2, wherein the amount ratio of the photocatalytic titanium dioxide, the acidified bentonite, the lauric acid monoglyceride, and the alcohol in step S1 is 10 g: 2.3-2.8 g: 1.5-1.7 g: 40-45mL, wherein the alcohol is reagent grade alcohol, and the alcohol concentration is 95%.
6. The preparation method of the wide-temperature selective adsorption displacement desulfurization material according to claim 2, wherein the dosage ratio of the emulsified base material to the deionized water is 1 mL: 3.5-4 mL.
7. The method for preparing the wide-temperature selective adsorption displacement desulfurization material according to claim 2, wherein the pH adjustment in the steps A1 and S2 is performed by using sodium hydroxide solution, and the mass fraction of the sodium hydroxide solution is 12% -15%.
8. The method for preparing the wide-temperature selective adsorption displacement desulfurization material according to claim 1, wherein the transition metal oxide is one of calcium oxide, sodium oxide, iron oxide and copper oxide.
9. The method for preparing the wide-temperature selective adsorption replacement desulfurization material according to claim 2, wherein the acidified bentonite is one of sodium-based acidified bentonite and calcium-based acidified bentonite.
10. The method for preparing a wide-temperature-selective adsorptive displacement desulfurization material according to claim 1, wherein the promoter is one of 3-methylthiazolidine-thione-2 and 1- (N-oxydiethylene thiocarbamoyl) -2- (N-oxydiethylene) thiobenzimidazole.
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