CN115970487A - Polymer resin denitration agent and preparation method thereof - Google Patents
Polymer resin denitration agent and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of flue gas denitration, and particularly relates to a high-molecular resin denitration agent and a preparation method thereof. The preparation method comprises the steps of impregnating, drying and roasting the catalyst and the heat stabilizer, then carrying out amino silane coupling agent grafting modification on the surface of the heat stabilizer containing the catalyst, and polymerizing urea or melamine or a mixture of urea and melamine and formaldehyde into amino polymer resin through polymerization, so that the thermal stability is improved, and the catalyst has better denitration performance; and an alkali metal promoter is added, so that adsorption and enrichment of NO on the surface of the high-molecular resin denitration agent are facilitated, and the denitration performance is further improved. The components of the polymer resin denitration agent prepared by the method comprise amino polymer resin, a catalyst, a heat stabilizer and an alkali metal promoter, and compared with urea and melamine, the polymer resin denitration agent has stronger heat resistance, can well improve the denitration performance, and is in a powdery state so as to be convenient for gas conveying and storage.
Description
Technical Field
The invention belongs to the technical field of flue gas denitration, and particularly relates to a high-molecular resin denitration agent and a preparation method thereof.
Background
Nitrogen oxides are polluting gases generated in various industrial processes of coal-fired power plants, refuse incineration, cement plants and the like, and have strong harm to the environment and human bodies. Currently, the most common NOx control methods are ammonia Selective Catalytic Reduction (SCR); the other is selective non-catalytic reduction (SNCR) using ammonia, aqueous urea. Although the SCR flue gas denitration technology has higher denitration efficiency, the SCR flue gas denitration technology has poor applicability to industries with complex flue gas components, such as waste incineration and the like, and mainly the flue gas contains a large amount of HCl and SO 2 And the like, and smoke with high Na, K and the like contents. Meanwhile, the fly ash particles erode the catalyst more seriously, and impurity metal ions are adsorbed on the surface of the catalyst to deactivate the catalyst. The selective non-catalytic reduction (SNCR) denitration technology refers to the process of using reducing agents such as ammonia to remove NO in flue gas at high temperature X Reduction to N 2 . The method has the greatest advantages that the cost is lower, but the SNCR denitration efficiency is lower, meanwhile, when ammonia is used as a reducing agent, the transportation and storage of liquid ammonia have high safety protection requirements, the denitration process of the ammonia water and the urea solution has high energy consumption and lower efficiency, and the ammonia leakage in the ammonia and urea process easily causes the problem of secondary pollution.
The PNCR denitration technology is characterized in that a high-molecular denitration agent is heated and decomposed under a high temperature (850-1200 ℃) condition to generate active ammonia and a reducing group, the active ammonia and the reducing group react with NO in flue gas to generate substances such as nitrogen, carbon dioxide and water which do not pollute the environment, and therefore the purpose of denitration is achieved. Therefore, the thermal decomposition performance of the denitration agent is crucial to the denitration performance, excessive ammonia gas can be decomposed due to the fact that urea is decomposed too fast at the high temperature when the nozzle is blocked, and accordingly unreacted ammonia gas is oxidized to generate NO, the use ratio of the denitration agent is low, and the denitration efficiency is poor. Chinese patent publication No. CN 108187490a discloses a polymeric dry denitration agent, which simply grinds and mixes a reducing agent including urea, and does not fundamentally solve the decomposition problem. Chinese patent publication No. CN 114272752a provides an organic coated denitration agent and a preparation method thereof, which performs surface modification on the surface of urea molding particles in a coating manner to form a polyurethane polymer film, thereby improving the heat resistance thereof, effectively slowing the ineffective decomposition of urea at a denitration temperature, and improving the utilization rate of urea. However, this method does not improve the thermal decomposition performance of urea itself, and urea is decomposed at a low temperature and diffuses out of the polymer film.
Disclosure of Invention
One of the purposes of the invention is to provide a preparation method of a high polymer resin denitration agent, and the high polymer resin denitration agent prepared by the method has excellent heat resistance and high denitration efficiency, and meanwhile, has good powder fluidity and is convenient to store, transport and convey.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a polymer resin denitration agent comprises the following steps:
s1, adding 0.1-20 parts by mass of a catalyst precursor into 50 parts by mass of water to prepare an aqueous solution, adding 1-30 parts by mass of a heat stabilizer, stirring, impregnating, drying, calcining at 300-600 ℃, and grinding to obtain solid powder;
s2, adding 1-10 parts by mass of amino silane coupling agent into an ethanol water solution, pre-hydrolyzing, adding all solid powder prepared in the step S1, stirring at room temperature for full reaction, centrifuging, washing and drying to prepare a heat stabilizer containing a catalyst;
s3, adding 40-500 parts by mass of formaldehyde aqueous solution into a reaction kettle, wherein the concentration of the formaldehyde aqueous solution is 10-50wt%, stirring and heating to 40-95 ℃ and keeping the temperature, sequentially adding 30-90 parts by mass of melamine or urea, 1-10 parts by mass of surfactant and 1.1-50 parts by mass of the heat stabilizer containing the catalyst prepared in the step S2, adjusting the pH value of the solution to 4-12, reacting for 1.5-2h, cooling, carrying out suction filtration and drying on a reaction product, and obtaining a solid high molecular product containing the amino high molecular resin;
or adding 40-500 parts by mass of formaldehyde aqueous solution into a reaction kettle, wherein the concentration of the formaldehyde aqueous solution is 10-50wt%, stirring and heating to 60-95 ℃ and keeping the temperature, adding 30-90 parts by mass of melamine and 30-90 parts by mass of urea, adding 1-5 parts by mass of 10wt% sodium hydroxide solution, stirring and reacting for 1.5-2h, sequentially adding 1-10 parts by mass of surfactant and 1.1-50 parts by mass of heat stabilizer containing the catalyst prepared in the step S2, cooling to 40-50 ℃, adjusting the pH value of the solution to 4-12, heating to 60-90 ℃, continuing to react for 1.5-2h, cooling, and carrying out suction filtration and drying on the reaction product to obtain a solid polymer product containing amino polymer resin;
and S4, taking 100 parts by mass of the solid polymer product prepared in the step S3, adding 1-20 parts by mass of an alkali metal promoter, mixing, and grinding to obtain the polymer resin denitration agent.
The preparation method of the polymer resin denitration agent is further improved as follows:
preferably, the catalyst precursor is one or a combination of more than two of nitrate, acetate, oxalate and acetylacetone of iron, manganese and copper.
Preferably, the heat stabilizer is one or a combination of more than two of alumina, kaolin, attapulgite, montmorillonite, diatomite and bentonite.
Preferably, the amino silane coupling agent is one or a combination of two or more of KH-540, KH-550 and KH-792.
Preferably, the surfactant is one or a combination of more than two of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and sodium dodecyl sulfonate.
Preferably, the alkali metal promoter is one or more of sodium carbonate, sodium hydroxide, calcium oxide, calcium carbonate and calcium acetylacetonate.
Preferably, the amine-based polymer resin is one or a combination of two or more of melamine-formaldehyde resin, melamine-formaldehyde-urea resin and urea-formaldehyde resin.
Preferably, the ethanol aqueous solution in the step S2 is 30-50 parts by mass, and the concentration of the ethanol aqueous solution is 30-85wt%.
Preferably, the pH value of the formic acid added in the step S3 is adjusted to 4-12.
The invention also aims to provide the polymer resin denitration agent prepared by any one of the preparation methods.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention provides a preparation method of a polymer resin denitration agent, which specifically comprises the steps of S1-S4, wherein after a catalyst and a heat stabilizer are soaked, dried and roasted in the step S1, the heat stabilizer and the surface of the catalyst are subjected to amino silane coupling agent grafting modification in the step S2 to obtain the surface-modified heat stabilizer containing the catalyst, the dispersibility of the surface-modified heat stabilizer in resin can be improved, the resin polymerization is not influenced, the added heat stabilizer can slow down the decomposition of the denitration agent at high temperature, and the denitration agent is prevented from being accumulated at a spray gun opening. The added catalyst can improve the denitration efficiency; in the step S3, urea or melamine or a mixture of urea and melamine and formaldehyde are polymerized into amino polymer resin through polymerization, the amino polymer resin is one or a combination of more than two of melamine-formaldehyde polymer resin, melamine-formaldehyde-urea polymer resin and urea-formaldehyde polymer resin, so that the thermal stability is improved, the denitration performance is better, and the synthesized resin is powdery and is convenient for gas transportation and storage; in the step S4, the alkali metal promoter is added, so that adsorption and enrichment of NO on the surface of the high polymer resin denitration agent are facilitated, and the denitration performance is further improved.
2) The components of the polymer resin denitration agent prepared by the method comprise amino polymer resin, a catalyst, a heat stabilizer and an alkali metal promoter, and compared with urea and melamine, the polymer resin denitration agent has stronger heat resistance and can well improve the denitration performance, and the synthesized denitration agent is powdery and is convenient for gas transportation and storage. The denitration agent disclosed by the invention is simple in formula and low in cost.
Drawings
FIG. 1 is a thermogravimetric comparison graph of polymer resin denitrifiers 1 and 6, melamine and urea prepared in examples 1 and 6 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative effort based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of a polymer resin denitration agent 1, which specifically comprises the following steps:
s1, adding 20 parts by mass of ferric nitrate into 50 parts by mass of water to prepare an aqueous solution, adding 10 parts by mass of kaolin, stirring, impregnating, drying, calcining at a high temperature of 400 ℃, and grinding to obtain solid powder;
s2, adding 2 parts by mass of amino silane coupling agent KH-550 into 30 parts by mass of 30wt% ethanol aqueous solution, pre-hydrolyzing, adding all solid powder prepared in the step S1, stirring at room temperature for full reaction, centrifuging, washing with acetone, and drying to obtain a heat stabilizer containing a catalyst;
s3, adding 140 parts by mass of 10wt% aqueous formaldehyde solution into a reaction kettle, stirring and heating to 80 ℃ and keeping the temperature, then sequentially adding 62 parts by mass of melamine, 4 parts by mass of surfactant sodium dodecyl benzene sulfonate and 10 parts by mass of the catalyst-containing heat stabilizer prepared in the step S2, finally adding formic acid to adjust the reaction pH to 4, reacting for 1.5h, cooling, carrying out suction filtration and drying on the reaction product, and obtaining a solid polymer product containing amino polymer resin;
and S4, taking 100 parts by mass of the solid polymer product containing the amino polymer resin prepared in the step S3, adding 10 parts by mass of calcium oxide, mixing and grinding to obtain the polymer resin denitration agent 1.
Example 2
The embodiment provides a preparation method of a polymer resin denitration agent 2, which specifically comprises the following steps:
s1, adding 0.1 part by mass of copper acetylacetonate into 50 parts by mass of water to prepare an aqueous solution, adding 15 parts by mass of attapulgite, stirring, impregnating, drying, calcining at a high temperature of 500 ℃, and grinding to prepare solid powder;
s2, adding 5 parts by mass of amino silane coupling agent KH-540 into 30 parts by mass of 80wt% ethanol aqueous solution, pre-hydrolyzing, adding all solid powder prepared in the step S1, stirring at room temperature for full reaction, centrifuging, washing with acetone, and drying to obtain a heat stabilizer containing a catalyst;
s3, adding 140 parts by mass of 50wt% formaldehyde aqueous solution into a reaction kettle, stirring and heating to 85 ℃ and keeping the temperature, then sequentially adding 78 parts by mass of melamine, 5 parts by mass of surfactant sodium dodecyl benzene sulfonate and 50 parts by mass of catalyst-containing heat stabilizer prepared in the step S2, finally adding formic acid to adjust the reaction pH to 5, reacting for 1.5h, cooling, and carrying out suction filtration and drying on the reaction product to obtain a solid polymer product containing amino polymer resin;
and S4, taking 100 parts by mass of the solid polymer product containing the amino polymer resin prepared in the step S3, adding 15 parts by mass of calcium hydroxide, mixing and grinding to obtain the polymer resin denitration agent 2.
Example 3
The embodiment provides a preparation method of a polymer resin denitration agent 3, which specifically comprises the following steps:
s1, firstly, adding 17 parts by mass of iron acetate into 50 parts by mass of water to prepare an aqueous solution, then adding 30 parts by mass of montmorillonite, stirring, impregnating, drying, calcining at a high temperature of 600 ℃, and grinding to prepare solid powder;
s2, adding 5 parts by mass of an amino silane coupling agent KH-550 into 35 parts by mass of a 50wt% ethanol aqueous solution, performing prehydrolysis, adding all solid powder prepared in the step S1, stirring at room temperature to react fully, centrifuging, washing with acetone, and drying to obtain a heat stabilizer containing a catalyst;
s3, adding 262 parts by mass of 37wt% formaldehyde aqueous solution into a reaction kettle, stirring and heating to 75 ℃ and keeping the temperature, adding 75 parts by mass of urea, 38 parts by mass of melamine and 1 part by mass of 10wt% NaOH solution, stirring and reacting for 1.5 hours, sequentially adding 2 parts by mass of sodium dodecyl benzene sulfonate and 40 parts by mass of the catalyst-containing heat stabilizer prepared in the step S2, cooling to 50 ℃, adding formic acid to adjust the pH value to 5.5, heating to 60 ℃, continuing to react for 2 hours, cooling, carrying out suction filtration and drying on a reaction product, and obtaining a solid polymer product containing the amino polymer resin;
and S4, taking 100 parts by mass of the solid polymer product containing the amino-based polymer resin prepared in the step S3, adding 5 parts by mass of sodium hydroxide, mixing, and grinding to obtain the polymer resin denitration agent 3.
Example 4
The embodiment provides a preparation method of a polymer resin denitration agent 4, which specifically comprises the following steps:
s1, firstly, adding 1 part by mass of manganese nitrate into 50 parts by mass of water to prepare an aqueous solution, then adding 30 parts by mass of diatomite, stirring, impregnating, drying, calcining at a high temperature of 550 ℃, and grinding to obtain solid powder;
s2, adding 4 parts by mass of amino silane coupling agent KH-550 into 40 parts by mass of 45wt% ethanol aqueous solution, pre-hydrolyzing, adding all solid powder prepared in the step S1, stirring at room temperature for full reaction, centrifuging, washing with acetone, and drying to obtain a heat stabilizer containing a catalyst;
s3, adding 500 parts by mass of 44wt% formaldehyde aqueous solution into a reaction kettle, stirring and heating to 85 ℃ and keeping the temperature, adding 90 parts by mass of urea, 90 parts by mass of melamine and 2 parts by mass of 10wt% NaOH solution, stirring and reacting for 1.5 hours, sequentially adding 6 parts by mass of sodium dodecyl benzene sulfonate and 40 parts by mass of the catalyst-containing heat stabilizer prepared in the step S2, cooling to 40 ℃, adding formic acid to adjust the pH value to 5, heating to 60 ℃, continuing to react for 2 hours, cooling, carrying out suction filtration and drying on a reaction product, and obtaining a solid polymer product containing the amino polymer resin;
and S4, taking 100 parts by mass of the solid polymer product containing the amino polymer resin prepared in the step S3, adding 25 parts by mass of sodium carbonate, mixing, and grinding to obtain the polymer resin denitration agent 4.
Example 5
The embodiment provides a preparation method of a polymer resin denitration agent 5, which specifically comprises the following steps:
s1, firstly, adding 20 parts by mass of copper nitrate into 50 parts by mass of water to prepare an aqueous solution, then adding 25 parts by mass of bentonite, stirring, impregnating, drying, calcining at a high temperature of 600 ℃, and grinding to obtain solid powder;
s2, adding 10 parts by mass of amino silane coupling agent KH-792 into 35 parts by mass of 70wt% ethanol aqueous solution, pre-hydrolyzing, adding all solid powder prepared in the step S1, stirring at room temperature for full reaction, centrifuging, washing with acetone, and drying to obtain a heat stabilizer containing a catalyst;
s3, adding 303 parts by mass of 25wt% formaldehyde aqueous solution into a reaction kettle, stirring and heating to 70 ℃, keeping the temperature, then sequentially adding 85 parts by mass of urea, 5 parts by mass of sodium dodecyl benzene sulfonate and 10 parts by mass of the heat stabilizer containing the catalyst prepared in the step S2, adding formic acid to adjust the pH value to 5, reacting for 2 hours, cooling to room temperature, and drying in a drying oven to obtain a solid polymer product containing amino polymer resin;
and S4, taking 100 parts by mass of the solid polymer product containing the amino polymer resin prepared in the step S3, adding 5 parts by mass of calcium acetylacetonate, mixing, and grinding to obtain the polymer resin denitration agent 5.
Example 6
The embodiment provides a preparation method of a polymer resin denitration agent 6, which specifically comprises the following steps:
s1, firstly adding 9 parts by mass of manganese acetate into 50 parts by mass of water to prepare an aqueous solution, then adding 30 parts by mass of kaolin, stirring, impregnating, drying, calcining at a high temperature of 450 ℃, and grinding to prepare solid powder;
s2, adding 8 parts by mass of an amino silane coupling agent KH-540 into 35 parts by mass of 85wt% ethanol aqueous solution, pre-hydrolyzing, adding all solid powder prepared in the step S1, stirring and reacting at room temperature for 20 hours, centrifuging, washing with acetone, and drying to obtain a heat stabilizer containing a catalyst;
s3, adding 262 parts by mass of 30wt% formaldehyde aqueous solution into a reaction kettle, stirring and heating to 85 ℃ and keeping the temperature, adding 89 parts by mass of urea, 4 parts by mass of sodium dodecyl benzene sulfonate and 5 parts by mass of the heat stabilizer containing the catalyst prepared in the step S2, adding formic acid to adjust the pH value to 5.5, reacting for 1.5h, cooling, and carrying out suction filtration and drying on a reaction product to obtain a solid polymer product containing amino polymer resin;
and S4, adding 20 parts by mass of calcium hydroxide into 100 parts by mass of the solid polymer product prepared in the step S3, mixing, and grinding to obtain the polymer resin denitration agent 6.
FIG. 1 is a thermogravimetric comparison graph of polymer resin denitrifiers 1 and 6 prepared in examples 1 and 6 of the present invention with melamine and urea alone. As is clear from fig. 1, the heat resistance is significantly improved by the polymer having a crosslinked structure formed after polymerization.
Comparative example 1
Comparative example 1 is a melamine-formaldehyde resin, which was prepared according to example 2, except that: in step S3, 50 parts by mass of the catalyst-containing heat stabilizer prepared in step S2 is not added, and the melamine-formaldehyde resin is finally prepared.
Comparative example 2
Comparative example 2 is a melamine-urea-formaldehyde resin, which was prepared according to example 3, with the following exceptions: in step S3, "40 parts by mass of the catalyst-containing heat stabilizer prepared in step S2 is not added", and the melamine-urea-formaldehyde resin is finally prepared.
Comparative example 3
Comparative example 2 is a urea-formaldehyde resin, which was prepared according to example 5, except that: in step S3, 10 parts by mass of the catalyst-containing heat stabilizer obtained in step S2 is not added, and the urea-formaldehyde resin is finally obtained.
The denitration performance of the denitration agent was evaluated by passing the agent through a denitration performance evaluation apparatus comprising a fixed bed reaction apparatus and an on-line analyzer, and the denitration performance of examples 1 to 6 was evaluated at 800 to 900 ℃. Table 1 shows the denitration rates obtained at different temperatures for examples 1 to 6 at a NO concentration of 500 ppm.
TABLE 1 Performance test results of different amine-based polymeric resin denitrifiers
From the test results in table 1, it can be seen that when urea and melamine were used as the denitration agent without treatment, the denitration rates were only 45% and 32%, while the denitration rates of the polymer resin synthesized by the present invention were all above 90%.
Comparative examples 1, 2 and 3 are polymer resin denitrifiers without additives, and all of them have denitration rates of 90% or less.
The thermogravimetric characterization in fig. 1 shows that the weight loss temperature (370 ℃) of example 1 is remarkably increased relative to melamine (300 ℃), the weight loss temperature (300 ℃) of example 6 is also remarkably improved relative to urea (210 ℃), and the corresponding denitration rate is greatly increased compared with melamine and urea.
The above are only preferred embodiments of the present invention, and do not limit the scope of the present invention, and it is obvious to those skilled in the art that various modifications and variations can be made in the present invention. Changes and modifications to the above-described embodiments are intended to fall within the scope of the appended claims, as fall within the true spirit of the invention.
Claims (10)
1. The preparation method of the polymer resin denitration agent is characterized by comprising the following steps:
s1, adding 0.1-20 parts by mass of a catalyst precursor into 50 parts by mass of water to prepare an aqueous solution, adding 1-30 parts by mass of a heat stabilizer, stirring, impregnating, drying, calcining at 300-600 ℃, and grinding to obtain solid powder;
s2, adding 1-10 parts by mass of an amino silane coupling agent into an ethanol water solution, pre-hydrolyzing, adding all solid powder prepared in the step S1, stirring at room temperature to react fully, centrifuging, washing and drying to prepare a heat stabilizer containing a catalyst;
s3, adding 40-500 parts by mass of formaldehyde aqueous solution into a reaction kettle, wherein the concentration of the formaldehyde aqueous solution is 10-50wt%, stirring and heating to 40-95 ℃ and keeping the temperature, sequentially adding 30-90 parts by mass of melamine or urea, 1-10 parts by mass of surfactant and 1.1-50 parts by mass of the heat stabilizer containing the catalyst prepared in the step S2, adjusting the pH value of the solution to 4-12, reacting for 1.5-2h, cooling, carrying out suction filtration and drying on a reaction product, and obtaining a solid high molecular product containing the amino high molecular resin;
or adding 40-500 parts by mass of formaldehyde aqueous solution into a reaction kettle, wherein the concentration of the formaldehyde aqueous solution is 10-50wt%, stirring and heating to 60-95 ℃ and keeping the temperature, adding 30-90 parts by mass of melamine and 30-90 parts by mass of urea, adding 1-5 parts by mass of 10wt% sodium hydroxide solution, stirring and reacting for 1.5-2h, sequentially adding 1-10 parts by mass of surfactant and 1.1-50 parts by mass of heat stabilizer containing the catalyst prepared in the step S2, cooling to 40-50 ℃, adjusting the pH value of the solution to 4-12, heating to 60-90 ℃, continuing to react for 1.5-2h, cooling, and carrying out suction filtration and drying on the reaction product to obtain a solid polymer product containing amino polymer resin;
and S4, taking 100 parts by mass of the solid polymer product prepared in the step S3, adding 1-20 parts by mass of an alkali metal promoter, mixing, and grinding to obtain the polymer resin denitration agent.
2. The method for preparing a polymer resin denitration agent according to claim 1, wherein the catalyst precursor is one or a combination of two or more of nitrates, acetates, oxalates, and acetylacetonates of iron, manganese, and copper.
3. The method of claim 3, wherein the heat stabilizer is one or a combination of two or more of alumina, kaolin, attapulgite, montmorillonite, diatomaceous earth, and bentonite.
4. The method of claim 1, wherein the aminosilane coupling agent is one or a combination of two or more of KH-540, KH-550 and KH-792.
5. The method for preparing a polymer resin denitration agent according to claim 1, wherein the surfactant is one or a combination of two or more of sodium dodecylbenzene sulfonate, sodium dodecyl sulfate and sodium dodecyl sulfate.
6. The method for preparing a polymer resin denitration agent according to claim 1, wherein the alkali metal promoter is one or more of sodium carbonate, sodium hydroxide, calcium oxide, calcium carbonate and calcium acetylacetonate.
7. The method of claim 1, wherein the amine-based polymer resin is one or a combination of two or more of melamine-formaldehyde resin, melamine-formaldehyde-urea resin, and urea-formaldehyde resin.
8. The method of claim 1, wherein the ethanol aqueous solution is 30 to 50 parts by mass and the concentration of the ethanol aqueous solution is 30 to 85wt% in step S2.
9. The method of claim 1, wherein the formic acid is added to adjust the pH of the solution to 4 to 12 in step S3.
10. A polymer resin denitration agent prepared by the preparation method of any one of the preceding claims.
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