CN117772205B - Preparation method and application of activated coke-based solid waste resource modification catalyst - Google Patents
Preparation method and application of activated coke-based solid waste resource modification catalyst Download PDFInfo
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- CN117772205B CN117772205B CN202311780585.9A CN202311780585A CN117772205B CN 117772205 B CN117772205 B CN 117772205B CN 202311780585 A CN202311780585 A CN 202311780585A CN 117772205 B CN117772205 B CN 117772205B
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- 238000012986 modification Methods 0.000 title claims abstract description 13
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- -1 polypropylene Polymers 0.000 claims description 25
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
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- 229910017052 cobalt Inorganic materials 0.000 claims description 4
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 2
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- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 2
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- Catalysts (AREA)
Abstract
本发明公开了一种活性焦基固废资源化改性催化剂的制备方法，属于污水处理技术领域。本发明所述的一种活性焦基固废资源化改性催化剂的制备方法包括以下步骤：1）活性焦及可进行资源化回收利用的固废材料进行研磨、筛分；2）过筛物进行酸洗、去离子水浸泡清洗，去除杂质后烘干备用；3）烘干后物质进行金属活性物负载；4）混合物热解处理，得到活性焦基固废资源化改性催化剂。改性后的催化剂催化活性和催化效率得到有效提高，具备了更加稳定的表面结构，使用周期得到有效延长，同时实现了固废材料的资源化，有助于改善焦化废水高级氧化处理中臭氧利用率低、催化剂成本高的技术瓶颈。The present invention discloses a method for preparing an activated coke-based solid waste resource modification catalyst, and belongs to the technical field of sewage treatment. The method for preparing an activated coke-based solid waste resource modification catalyst described in the present invention comprises the following steps: 1) grinding and screening activated coke and solid waste materials that can be recycled and utilized; 2) acid washing and deionized water soaking and cleaning the sieved materials, drying for standby after removing impurities; 3) loading metal active substances on the dried materials; 4) pyrolysis treatment of the mixture to obtain an activated coke-based solid waste resource modification catalyst. The catalytic activity and catalytic efficiency of the modified catalyst are effectively improved, and it has a more stable surface structure, and the service life is effectively extended. At the same time, the resource utilization of solid waste materials is realized, which helps to improve the technical bottlenecks of low ozone utilization and high catalyst cost in the advanced oxidation treatment of coking wastewater.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a preparation method and application of an active coke-based solid waste recycling modified catalyst.
Background
The ozone oxidation technology has the advantages of simple operation condition, good treatment effect and short treatment period, and is widely applied to the treatment of high-concentration COD sewage in the chemical industries such as coking wastewater, papermaking wastewater, pharmaceutical wastewater and the like. After the ozone catalytic oxidation catalyst is introduced, the oxidation potential of ozone is obviously improved, the generated ozone can reduce the reaction activation energy or change the reaction process, various free radicals with higher activity and lower selectivity than ozone, such as hydroxyl free radicals, can be induced to decompose, and the macromolecule removal rate and the micromolecule mineralization rate can be effectively improved.
The common ozone oxidation catalysts are three types, mainly carrier materials with higher mechanical strength, such as ceramsite, aluminum oxide and the like; metal oxides having relatively high activity such as manganese dioxide, zinc oxide, and titanium dioxide; porous materials with excellent adsorption performance such as active carbon, zeolite, active coke and the like. The active coke has a micropore and mesopore structure, the specific surface area is about 600-1000 m 2/g, the adsorption rate is high, the selective adsorption capacity is high, and the cost is low. Related researches show that the aperture distribution of the active coke has higher matching property with the molecular diameter of refractory organic matters in the biochemical tail water of the coking wastewater, and has wide application prospect in the treatment of the coking wastewater. However, compared with other catalytic materials, active coke has the limitations of unstable structure and limited catalytic effect.
In recent years, plastic products are increasingly frequently used, such as polypropylene plastic capable of resisting high temperature of 100 ℃, and the polypropylene plastic is also an important raw material for manufacturing disposable protective clothing and disposable masks besides being applied to the fields of food packaging, household articles, automobiles, optical fibers and the like. With the development of related industries, waste polypropylene plastics become one of solid waste high polymer materials with larger yield in recent years, and the recycling treatment requirement of polypropylene plastics is also more urgent.
Aiming at the technical background, the invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which are used for mixing and modifying active coke and recycled polyethylene plastic to form a new ozone catalyst which is applied to the catalytic oxidation treatment of coking wastewater, and simultaneously, the removal efficiency is improved, the preparation cost is reduced, the solid waste materials are recycled, and the transformation requirements of the current energy-saving carbon reduction treatment of the coking wastewater are met.
Disclosure of Invention
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which is characterized by comprising the following steps: 1) Grinding and screening active coke and solid waste materials; 2) Soaking and cleaning the screened material, and drying; 3) Carrying out impregnated metal loading on the dried material; 4) Calcining the mixture to obtain the active coke carrier resource modified catalyst.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which is characterized in that active coke, shells, coconut shells, polyvinyl chloride plastics, polypropylene plastics and the like are ground and then screened by a 100-mesh screen, preferably, the solid waste material is selected as waste polypropylene plastics, and the mass ratio of the active coke to the polypropylene plastics is preferably 55% -80%: 20% -45%.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which are characterized in that 1 mol/L and 0.1 mol/L nitric acid are used for removing impurities after active coke and polypropylene plastics are screened, the active coke and the polypropylene plastics are soaked in deionized water and washed for 30-120 min after pickling, supernatant is removed, and washing is repeated for 2-3 times until no obvious impurities exist, and the pH value is near neutral. Preferably, the cleaning can be carried out for 30-60 min under the assistance of ultrasound.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which is characterized in that cleaned active coke and polypropylene plastic are dried in a vacuum drying oven at 60-120 ℃, preferably in a vacuum drying oven at 80-100 ℃, and air is isolated in a drying vessel for cooling.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which is characterized in that a mixture after cleaning and drying is immersed into a metal nitrate solution with a certain concentration, wherein the metal nitrate solution is one or more of manganese, cerium, iron, nickel and cobalt nitrate solutions, and the loading mass fraction of metal active components is 2% -15%. Preferably, the impregnating solution is prepared by mixing ferric nitrate, cobalt nitrate and nickel nitrate in a mass fraction ratio of about iron: cobalt: nickel=45% ≡55% >: 25% -30%: 20% -25%. The dipping time is 24-96 hours, preferably 60-72 hours.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which is characterized in that a certain concentration of adhesive is added into a metal salt solution, so that the mechanical strength and the structural stability of the active coke and waste polypropylene plastic modified catalyst can be improved.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which are characterized in that a material is subjected to heat treatment in a 400-900 ℃ nitrogen protection tube furnace for 2-6 hours after being immersed, so that the active coke carrier-based recycling modified catalyst is obtained. The pyrolysis treatment temperature is preferably 700-900 ℃, the heating rate is 10 ℃/min, and the reaction time is preferably 2-4 h.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which is characterized in that the recycling modified catalyst can be applied to ozone catalytic oxidation treatment of coking wastewater and biochemical sewage with higher COD concentration, the catalytic activity and catalytic efficiency of the modified material are higher, the structural stability is higher, the recycling treatment of waste polypropylene plastic is realized, and the preparation cost of the catalyst is reduced.
The invention provides a preparation method and application of an active coke-based solid waste recycling modified catalyst, which are characterized in that the ratio of an oxidant, namely ozone to COD is about 1-2.5:1, and the addition amount of the catalyst is about 20% -30%.
Based on the above summary, the present invention has the following beneficial effects:
The active coke-based solid waste recycling modified catalyst provided by the invention has obvious advantages in the aspects of improving the catalytic efficiency and promoting the generation of hydroxyl radicals. The loaded active metal component can effectively improve the generation amount of hydroxyl free radicals on the surface of the catalyst, and simultaneously achieves the two purposes of improving the ozone utilization rate and the oxidizing property, thereby improving the oxidation performance and the oxidation efficiency of the whole ozone. The active coke has a relatively good specific surface area, can promote more metal active matters to be loaded on the outer surface of the material, increases the contact area of the metal active matters with ozone and pollutants, and strengthens the catalytic oxidation effect of the ozone.
The active coke-based solid waste recycling modified catalyst provided by the invention has obvious selection advantages. Compared with the common silicon-aluminum-based catalyst, the active coke carrier used in the invention has better adsorption performance, the aperture is more matched with molecules in the coking wastewater, and the pollution and blockage condition of anions and cations in the coking wastewater to the catalyst pore can be effectively improved. Compared with the adsorption materials such as activated carbon and the like with good adsorption performance, the invention has low cost, and on the basis of further reducing the preparation cost of the catalyst, a new thought is provided for the recycling treatment of the waste polypropylene plastics widely used in recent years due to doping of the waste polypropylene plastics with a certain proportion, and the invention meets the development requirements of pollution reduction, carbon reduction and resource recycling.
The active coke-based solid waste recycling modified catalyst provided by the invention has obvious advantages in the aspect of reducing the preparation cost of the catalyst. The loaded metal active substances are tightly loaded on the outer surface of the material under the auxiliary action of the adhesive, so that the mechanical strength of the catalyst is effectively increased, and the stability of the catalyst is enhanced; the service cycle of the catalyst is effectively prolonged, the catalyst can play a role stably for a long time, and the trouble of replacing the catalyst and the economic cost caused by the trouble are reduced.
Drawings
FIG. 1 is a graph showing the comparison of the effect of the modified catalyst for treating oxalic acid solution based on different solid waste materials of active coke carriers.
Fig. 2 shows the experimental effect of recycling the modified catalyst based on the active coke carrier.
Description of the embodiments
According to the preparation method and application of the active coke-based solid waste recycling modified catalyst, compared with active coke, the recycling modified catalyst has higher catalytic activity and catalytic efficiency, the adhesive improves the structural stability of the catalyst, prolongs the service cycle of the catalyst, realizes recycling treatment of solid waste materials, and reduces the preparation cost of the catalyst. The specific embodiments are as follows.
A preparation method and application of an active coke-based solid waste recycling modified catalyst are characterized in that the carrier material is a mixture of active coke and a recycling solid waste material, such as a shell, a coconut shell, polyethylene plastic, polyvinyl chloride plastic, polypropylene plastic and the like. Preferably, the solid waste material is selected from waste polypropylene plastics, and the mass ratio of active coke to polypropylene plastics is preferably 55% -80%: 20% -45%, and the preparation method of the active coke-based solid waste recycling modified catalyst comprises the following specific operation steps: 1) Mixing and crushing active coke and polypropylene plastic, sieving, cleaning with high and low concentration nitric acid to remove impurities, and then washing with deionized water until the pH is near neutral; 2) Drying the cleaned mixture in a vacuum drying oven, and isolating air in a drying dish for cooling; 3) Placing the dried mixture into one or more nitrate solutions, and completing metal active matter loading treatment under the auxiliary action of an adhesive; preferably, the mass fraction ratio is about iron: cobalt: nickel=45% ≡55% >: 25% -30%: 20% -25%, and the soaking time can be 60-72 hours; 4) And placing the loaded material in a nitrogen-protected tubular furnace for heat treatment to obtain the activated active Jiao Ji solid waste resource modified catalyst.
The invention is further illustrated below with reference to examples.
Example 1
The preparation method and the application of the active coke-based solid waste recycling modified catalyst provided by the invention screen application effects of solid waste materials capable of being recycled. The recyclable solid waste material is selected from fruit shells, polyvinyl chloride plastics (Polyvinyl chloride, PVC) and Polypropylene Plastics (PP), and is subjected to catalyst modification treatment by taking active coke as a carrier under the same preparation condition. Oxalic acid is selected as the target pollutant in the experiment, and is one kind of carboxylic acid and is often used as the target pollutant for judging the catalyst removal effect. The oxalic acid solution of 50 mg/L is treated by using the catalyst prepared from 100 mg/L of different recycling materials, the consistent condition is kept, the same temperature and pH are controlled, 5 mg/min ozone is introduced, sampling and detection are carried out at different times of the reaction, and the removal effect is shown in figure 1. Ozone alone will remove 76% of the oxalic acid, and "husk + ozone" and "PVC + ozone" will be similar in effect, with reaction 60 min removing 91% and 94% of the oxalic acid. The effect of the PP plus ozone is optimal, the removal rate of each sampling point is high, and finally 98 percent of oxalic acid can be removed. The application example shows that the modified catalyst based on active coke carrier recycling has good catalytic oxidation effect, and the polypropylene plastic is feasible as a preferable recycling material.
Example 2
The biochemical sewage of coking wastewater in a certain factory is compared and applied, and the experimental basic condition is that the pH is about 7, and the temperature is about 28 ℃ at room temperature. The COD of the inflow water can be reduced from 100 mg/L to 53.4 mg/L or so by using the common silicon-aluminum based catalyst, and the removal rate is about 46.6%. The catalyst dosage at this time was about 26.7% and the ozone concentration was 150 mg/L. The catalyst is used for treating the same-strand sewage, the using amount of the catalyst is 25%, the ozone concentration is 100 mg/L, the removal rate of 57.7% can be achieved, and the effluent concentration is as low as 42.3 mg/L. The two catalysts have limited ammonia nitrogen removal effect and have a certain effect on COD removal, and the removal rate of the modified catalyst based on active coke carrier recycling provided by the invention on COD is effectively improved.
Example 3
The catalytic material preference is evaluated by considering the reusable effect of the material, and the experiment is evaluated by 5 repeated treatment experiments aiming at coking actual wastewater. The experimental water is biochemical-coagulation effluent of a certain coking plant, and the experimental result is shown in figure 2. As can be seen from FIG. 2, the catalyst after the test can maintain a good ozone catalytic oxidation treatment effect when being used repeatedly for 5 times, the COD concentration difference of the effluent of the 5 times of experiments is not large, and the stable standard reaching of the COD of the biochemical-coagulation effluent quality of the coking wastewater can be ensured.
While the exemplary embodiments of the present invention have been described, the present invention is not limited to the above embodiments, and various modifications and changes can be made within the scope of the claims.
Claims (4)
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| CN103111290A (en) * | 2013-03-18 | 2013-05-22 | 哈尔滨工业大学 | Preparation method of catalyst for catalyzing ozonation for advanced treatment of coal chemical wastewater |
| CN115709052A (en) * | 2022-11-22 | 2023-02-24 | 上海交通大学 | Carbon nanotube modified sludge carbon material and preparation method and application thereof |
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| JPS5777019A (en) * | 1980-10-30 | 1982-05-14 | Toho Rayon Co Ltd | Fibrous activated carbon and its manufacture |
| JPH0631297A (en) * | 1992-07-10 | 1994-02-08 | Nippon Steel Corp | Advanced treatment method for wastewater containing high concentration nitrogen |
| CN102451711B (en) * | 2010-10-15 | 2013-06-19 | 中国石油化工股份有限公司 | Industrial wastewater treatment catalyst and preparation method thereof |
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