CN114250095B - Humic acid complex copper-based catalyst and preparation method and application thereof - Google Patents
Humic acid complex copper-based catalyst and preparation method and application thereof Download PDFInfo
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- CN114250095B CN114250095B CN202210051922.XA CN202210051922A CN114250095B CN 114250095 B CN114250095 B CN 114250095B CN 202210051922 A CN202210051922 A CN 202210051922A CN 114250095 B CN114250095 B CN 114250095B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L9/00—Treating solid fuels to improve their combustion
- C10L9/10—Treating solid fuels to improve their combustion by using additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L10/00—Use of additives to fuels or fires for particular purposes
- C10L10/02—Use of additives to fuels or fires for particular purposes for reducing smoke development
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/10—Complexes comprising metals of Group I (IA or IB) as the central metal
- B01J2531/16—Copper
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Abstract
The invention belongs to the technical field of coal chemical industry catalysts, and discloses a humic acid complex copper-based catalyst, and a preparation method and application thereof. The preparation method comprises the following preparation steps: (1) Dissolving weathered coal in water, fully stirring and dispersing, adding a certain amount of sodium hydroxide, stirring, mixing and reacting to obtain a solution A; (2) Dissolving sodium hydroxide and copper hydroxide in water, and fully and uniformly mixing to obtain a solution B; (3) And mixing the solution A and the solution B to obtain a mixed solution, stirring the mixed solution for reaction, and then performing spray drying to obtain the humic acid copper-based complex catalyst. The method can rapidly prepare the coal catalytic material with uniform particle size and high dispersion, in which CuO and humic acid are complexed, on a large scale through simple complexation of weathered coal and copper ions, and has the advantages of simple preparation process, low energy consumption and wide raw material source. Realizing high dispersion and large-scale preparation of the coal combustion catalyst.
Description
Technical Field
The invention belongs to the technical field of coal chemical industry catalysts, and particularly relates to a humic acid complex copper-based catalyst, and a preparation method and application thereof.
Background
The primary energy coal accounts for about 70% of energy consumption in China, coal accounting for about 80% of total coal production is used for direct combustion every year, and a small amount of high-added-value products are produced through the processes of pyrolysis, gasification, liquefaction and the like. Coal resources are mainly caused by low heat value utilization in the combustion process due to large heat capacity and difficult ignition and heat transfer. On the other hand, flame combustion is a traditional combustion mode of coal, the generated heat is not fully utilized, and the flame combustion is not fully combusted, so that energy waste is caused. Therefore, the coal is fully combusted, the combustion heat efficiency is improved, and the problem that heat energy workers need to overcome is solved.
The catalyst is added into the coal to enable the coal to be efficiently combusted, and the method is an effective measure for improving the combustion heat efficiency of the coal. The catalytic combustion technology can reduce the ignition temperature of coal, the combustion process is milder, and the oxygen concentration application range in combustion is wider, so that the method is one of the most effective methods for recycling energy at home and abroad at present.
Patent CN 104327905A discloses a preparation method of a coal combustion catalyst, which comprises the specific steps of adding triisopropanolamine, tertiary butanol, propylene glycol and isobutanol into a reaction kettle for stirring, adding alkali factory waste liquid, fully stirring and mixing, filtering, and then adding lanthanum nitrate, span-20, tween-20, naCl and FeCl 3 And heating the reaction kettle while continuously stirring, and reacting for a period of time to obtain the required coal combustion catalyst. The method can reduce ignition point of coal, increase combustion speed, improve coal combustion efficiency, and reduce harmful substance emission. However, in this method, a large hydrothermal reaction and an additional stirring and mixing device are required, and although the reaction substances can be effectively and sufficiently contacted with each other to promote the growth and crystallization of the catalyst and efficiently prepare the coal catalyst material, the catalyst crystals are seriously agglomerated in a high-temperature reaction kettle during the reaction process and have poor dispersibility. The intermediate product which does not completely participate in the reaction in the catalyst is gathered in the catalyst, the difficulty in purifying and separating the intermediate product is high, the content of the intermediate product is high, the purity of the material is low, the quality of the coal catalyst is seriously influenced, and the treatment cost of the catalyst is additionally added.
Patent CN 104371791A discloses a coal combustion catalyst, which is made from the following raw materials by weight percent: 13 to 22 percent of diethanol monoisopropanolamine, 25 to 35 percent of triethanolamine, 10 to 15 percent of nonionic surfactant, 13 to 20 percent of papermaking black liquor, 15 to 20 percent of sugar mill waste liquor, 1 to 6 percent of alkali metal salt and 0.2 to 0.8 percent of rare earth element compound. The ignition time is shortened by the diethanol monoisopropanolamine and the triethanolamine, and the combustion supporting effect is achieved; the black liquor contains a large amount of K 2 CO 3 、Na 2 CO 3 KOH, naOH and Ca (OH) 2 The catalyst is a coal-fired catalyst with good effect, can reduce the ignition temperature of coal, completely burn the coal, and has a desulfurization function; the sugar refinery waste liquid has stronger polarity, can reduce the combustion activation energy, and make the coal combustion become easy to carry out; alkali metal saltThe low ignition temperature can be changed, the burnout temperature is advanced, and the heat release of combustion can be increased; the compound of the rare earth element can promote the transfer of oxygen ions between the whole catalyst and coal particles, can obviously accelerate the combustion rate of coal, and reduces the activation energy of combustion reaction, thereby generating combustion-supporting effect. The patent also has the problems of poor dispersibility, high intermediate product content, low material purity and the like, and uses rare earth elements with higher price, so that the raw material cost is higher.
Patent CN 101497839A discloses a method for preparing composite catalyst fire coal, which improves the problems of the catalyst of the previous patent, and directly mixes and grinds the raw material of the catalyst and coal briquettes to obtain coal powder mixed with the catalyst. The raw materials do not need a hydrothermal reaction process, but the method needs crushing, grinding and screening processes, the process is complicated, the size of the catalyst particles on the prepared composite catalyst coal is uncontrollable, and the application range of the composite catalyst coal in the market with a plurality of high-quality coal catalysts is narrow. Therefore, it becomes important to develop a superior catalyst for application to catalytic combustion technology.
The highly dispersed copper-based catalytic material has the characteristics of high adsorption energy, high reaction active sites and the like, and is widely applied to the catalytic field. However, the decrease of catalytic activity and stability due to the small particle size, large surface energy and particle-to-particle agglomeration of the material limits the application of the dispersed nano-catalyst in industry. In order to improve the agglomeration phenomenon, the invention provides a weathered coal complexation method, and a method for preparing a high-dispersion copper-based catalyst for coal combustion by a simple stirring complexation process.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a preparation method of a humic acid complex copper-based catalyst.
The invention also aims to provide the humic acid complex copper-based catalyst prepared by the method.
The invention further aims to provide the application of the humic acid complex copper-based catalyst in coal combustion catalysis.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a humic acid complex copper-based catalyst comprises the following preparation steps:
(1) Dissolving weathered coal in water, fully stirring and dispersing, adding a certain amount of sodium hydroxide, stirring, mixing and reacting to obtain a solution A;
(2) Dissolving sodium hydroxide and copper hydroxide in water, and fully and uniformly mixing to obtain a solution B;
(3) And mixing the solution A and the solution B to obtain a mixed solution, stirring the mixed solution for reaction, and then performing spray drying to obtain the humic acid copper-based complex catalyst.
Further, the mass ratio of the weathered coal to the sodium hydroxide in the step (1) is 1.
Further, the mass ratio of the weathered coal to the water in the step (1) is 1.
Further, the temperature of the stirring mixing reaction in the step (1) is controlled to be 10-40 ℃, and the time is controlled to be 10-300 min.
Further, the mass ratio of the sodium hydroxide to the copper hydroxide added in the step (2) is 2-8:1.
Further, the mass ratio of the copper hydroxide to the water in the step (2) is 1.
Further, the temperature of the stirring reaction in the step (3) is controlled to be 5-65 ℃, and the time is controlled to be 5-100 h.
Further, the temperature of the spray drying in the step (3) is controlled to be 80-120 ℃.
The humic acid complex copper-based catalyst is prepared by the method.
The humic acid complex copper-based catalyst is applied to coal combustion catalysis.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method can rapidly prepare the coal catalytic material complexing CuO and humic acid on a large scale by simply complexing weathered coal and copper ions, and has the advantages of simple preparation process, low energy consumption and wide raw material source.
(2) The method can prepare the coal combustion catalyst with uniform and highly dispersed particle size, and realizes the high dispersion and large-scale preparation of the coal combustion catalyst.
Drawings
Fig. 1 is an X-ray (XRD) diagram of the highly dispersed humic acid complex copper-based catalyst prepared in example 1 of the present invention.
Fig. 2 is a low Transmission Electron Microscope (TEM) image of the highly dispersed humic acid complex copper-based catalyst prepared in example 1 of the present invention.
Fig. 3 is a high-power Transmission Electron Microscope (TEM) image of the highly dispersed humic acid complex copper-based catalyst prepared in example 1 of the present invention.
Fig. 4 is a selected area electron diffraction pattern (SAED) of the highly dispersed humic acid complex copper-based catalyst prepared in example 1 of the present invention.
Fig. 5 is a fourier infrared spectrum (FT-IR) of the highly dispersed humic acid complex copper-based catalyst prepared in example 1 of the present invention.
Fig. 6 is a thermogravimetric plot of a coal-feeding combustion catalyst sample and a raw coal sample obtained by adding the humic acid copper-based complex catalyst to raw coal in example 1 of the present invention.
FIG. 7 is a graph showing the burnout rate of a coal-added combustion catalyst sample and a raw coal sample obtained by adding the humic acid copper-based complex catalyst to raw coal in example 1 of the present invention.
Fig. 8 is a TEM image of the highly dispersed humic acid complex copper-based catalyst prepared in example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
The humic acid copper complex catalyst of the embodiment is prepared by the following method:
(1) 2g of weathered coal and 1g of sodium hydroxide were sequentially put into 60 ml of an aqueous solution, and the mixed solution was strongly stirred at room temperature for 40 minutes to obtain a solution A.
(2) 4g of sodium hydroxide and 2g of copper hydroxide are dissolved in 20 ml of water in sequence and are fully and uniformly mixed to obtain solution B.
(3) Solution B was slowly poured into solution A to give solution C. And stirring the solution C at 25 ℃ for reaction for 24 hours, and after the stirring reaction is finished, spray-drying the mixed solution at 85 ℃ to obtain the powdery humic acid complex copper-based catalyst with good dispersibility and dissolubility.
Fig. 1 is an XRD diffraction pattern of the copper-based humic acid catalyst obtained in this example, and it can be seen from the displayed image that the crystal structure of the material obtained in the present invention is a composite of CuO and carbon.
The morphology of the humic acid copper-based complex catalyst obtained in the embodiment is subjected to low-power TEM characterization analysis, and the analysis result is shown in FIG. 2, and it can be seen from FIG. 2 that the material prepared by the method of the present invention exhibits a well-dispersed morphology, does not significantly agglomerate, and exhibits uniform granular shapes.
The structure of the humic acid copper-based complex catalyst obtained in the embodiment is observed by a large-power TEM. As shown in fig. 3, it is understood from fig. 3 that the humic acid complex copper-based catalyst obtained by the method of the present invention is in a highly dispersed state, and no significant stacking is observed. The obtained CuO is a composite structure which is nano-particle of about 100nm and is uniformly loaded on the surface of the humic acid film.
Fig. 4 is a selected area electron diffraction pattern (SAED) of the copper-based humic acid complexed catalyst obtained in this embodiment, and it can be analyzed from the SAED picture that the catalyst prepared by the synthesis method of the present invention has a dark ring shape and exhibits obvious white and bright spots, which can indicate that the copper-based catalyst prepared by the method has a polycrystalline structure.
Fig. 5 is a fourier infrared spectrum (FT-IR) of the copper-based humic acid catalyst obtained in this example, from which it can be found that-OH and-NH functional groups of humic acid exist in the catalyst, and signals of Cu-O bond are also found, which indicates that humic acid is well complexed with metal.
Fig. 6 is thermogravimetric curves of a coal-adding combustion catalyst sample and a raw coal sample obtained by adding the humic acid copper-based complex catalyst obtained in the embodiment to raw coal. Fig. 7 is a burn-out rate curve of a coal-feeding combustion catalyst sample and a raw coal sample obtained by adding the humic acid copper-based complex catalyst obtained in the embodiment to raw coal, and it can be found from the graph that the burn-out time of the coal-feeding catalyst sample is shorter than that of the raw coal sample and the burn-out temperature is lower, and the two characteristics illustrate that the coal-feeding combustion catalyst has the characteristic of intensified combustion to coal after being added.
Example 2
The humic acid copper complex catalyst of the embodiment is prepared by the following method:
(1) 2g of weathered coal and 2g of sodium hydroxide were sequentially put into 70 ml of an aqueous solution, and the mixed solution was strongly stirred at room temperature for 120 minutes to obtain a solution A.
(2) 6g of sodium hydroxide and 2.5g of copper hydroxide are dissolved in 30 ml of water in sequence and are fully and uniformly mixed to obtain solution B.
(3) Solution B was slowly poured into solution A to give solution C. And stirring the solution C at 35 ℃ for reaction for 48 hours, and after the stirring reaction is finished, spray-drying the mixed solution at 120 ℃ to obtain the powdery humic acid complex copper-based catalyst with good dispersibility and dissolubility.
Fig. 8 is a TEM image of the powdery humic acid complexed copper-based catalyst with good dispersibility and solubility obtained in the present embodiment, and the obtained electron microscope image shows that the humic acid complexed copper-based catalyst obtained in the present invention is highly dispersed and uniform in morphology and size.
According to the results, the coal catalytic material which is formed by complexing CuO and humic acid and has uniform particle size and high dispersion can be rapidly prepared on a large scale by simply complexing weathered coal and metal ions by the method.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.
Claims (8)
1. The preparation method of the humic acid complex copper-based catalyst is characterized by comprising the following preparation steps of:
(1) Dissolving weathered coal in water, fully stirring and dispersing, adding a certain amount of sodium hydroxide, stirring, mixing and reacting to obtain a solution A;
(2) Dissolving sodium hydroxide and copper hydroxide in water, and fully and uniformly mixing to obtain a solution B;
(3) Mixing the solution A and the solution B to obtain a mixed solution, stirring the mixed solution for reaction, and then performing spray drying to obtain the humic acid copper-based complex catalyst;
the temperature of the stirring, mixing and reacting in the step (1) is controlled to be 10-40 ℃, and the time is controlled to be 10-300 min;
the mass ratio of the sodium hydroxide to the copper hydroxide in the step (2) is 2 to 8.
2. The preparation method of the humic acid copper-based complex catalyst according to claim 1, wherein the mass ratio of the weathered coal to the sodium hydroxide added in the step (1) is 1: 0.2: 4.
3. The preparation method of the humic acid copper-based complex catalyst according to claim 2, wherein the mass ratio of the weathered coal to water in the step (1) is 1 to 50 to 100.
4. The preparation method of the humic acid copper-based complex catalyst according to claim 1, wherein the mass ratio of the copper hydroxide to the water added in the step (2) is 1 to 10-30.
5. The preparation method of the humic acid copper-based complex catalyst according to claim 1, wherein the temperature of the stirring reaction in the step (3) is controlled to be 5 to 65 ℃, and the time is controlled to be 5 to 100 hours.
6. The method for preparing the copper-based humic acid complex catalyst according to claim 1, wherein the temperature of spray drying in the step (3) is controlled to be 80 to 120 ℃.
7. A humic acid copper complex catalyst prepared by the process of any one of claims 1~6.
8. The use of the copper complex humic acid catalyst as defined in claim 7 in coal combustion catalysis.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101289474A (en) * | 2008-06-25 | 2008-10-22 | 北京理工大学 | Process for preparing humic acid from residue after extraction of coal humic acid |
| CN109225336A (en) * | 2018-08-27 | 2019-01-18 | 内蒙古工业大学 | A kind of low-disintegration coal depolymerizing substance-copper-based catalysts and its preparation method and application |
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| JP4909457B2 (en) * | 2000-07-06 | 2012-04-04 | 三井造船株式会社 | Method for producing catalyst composition for iron hydroxide coal liquefaction |
| US20100044280A1 (en) * | 2006-01-24 | 2010-02-25 | Kimleigh Chemicals Sa (Pty) Ltd | Flotation Process Using an Organometallic Complex as Activator |
| US20090149324A1 (en) * | 2007-12-05 | 2009-06-11 | Basf Catalysts Llc | Low temperature water gas shift catalyst |
| WO2011054220A1 (en) * | 2009-11-03 | 2011-05-12 | Yin Xiaolin | Catalyst for coal combustion and method for multiphase dynamic catalytic oxidation combustion of coal dust |
| WO2015153520A1 (en) * | 2014-04-02 | 2015-10-08 | Georgia-Pacific Chemicals Llc | Methods for making lignocellulose composite products with oxidative binders and encapsulated catalyst |
| CN104028306B (en) * | 2014-06-09 | 2016-06-29 | 中国海洋石油总公司 | A kind of coal burning composite catalyst |
| CN109261368A (en) * | 2018-08-13 | 2019-01-25 | 昆明理工大学 | A kind of inhibitor and application method for magnetic iron ore |
| CN112169797B (en) * | 2020-10-14 | 2023-09-26 | 北京工业大学 | Preparation method of Cu-Fe bimetallic complex magnetic chitosan carbon aerogel catalyst applied to wet oxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289474A (en) * | 2008-06-25 | 2008-10-22 | 北京理工大学 | Process for preparing humic acid from residue after extraction of coal humic acid |
| CN109225336A (en) * | 2018-08-27 | 2019-01-18 | 内蒙古工业大学 | A kind of low-disintegration coal depolymerizing substance-copper-based catalysts and its preparation method and application |
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