CN108927118B - Petroleum coke calcination waste gas adsorbent and preparation method and application thereof - Google Patents
Petroleum coke calcination waste gas adsorbent and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01D2257/30—Sulfur compounds
- B01D2257/302—Sulfur oxides
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- B01D2257/702—Hydrocarbons
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- B01D2257/702—Hydrocarbons
- B01D2257/7022—Aliphatic hydrocarbons
Abstract
The invention provides a petroleum coke calcination waste gas adsorbent and a preparation method and application thereof, wherein the adsorbent comprises the following raw material components: activated carbon, coconut fibers, nano calcium carbonate, graphene and pentaerythritol. The active carbon is composed of coconut shell active carbon, sepiolite active carbon and apricot shell active carbon according to the mass ratio of 2:1: 3. The absorbent has the absorption rate of 95.3-96.7% for sulfur dioxide and 89.3-94.3% for nitrogen dioxide.
Description
Technical Field
The invention relates to a petroleum coke treatment method, and particularly relates to a petroleum coke calcination waste gas adsorbent, and a preparation method and application thereof.
Background
In the case of a graphite electrode for steel making or an anode paste (melting electrode) for aluminum or magnesium making, green coke must be calcined to meet the requirements for petroleum coke (green coke). The calcining temperature is generally about 1300 ℃, so that petroleum coke volatile components are removed as much as possible. Therefore, the hydrogen content of petroleum coke reworked products can be reduced, the graphitization degree of the petroleum coke is improved, the high-temperature strength and the heat resistance of the graphite electrode are improved, and the conductivity of the graphite electrode is improved. The calcined coke is mainly used for producing graphite electrodes, carbon paste products, diamond dust, food-grade phosphorus industry, metallurgical industry, calcium carbide and the like, wherein the graphite electrodes are most widely applied. The raw coke can be directly used as calcium carbide main material to produce silicon carbide and boron carbide as grinding material without calcining. It can also be used directly as coke for blast furnace in metallurgical industry or as brick for lining carbon on blast furnace wall, or as dense coke for casting process. During the process of calcining green coke into calcined coke, a large amount of flue gas is generated, and the flue gas contains pollutants mainly comprising sulfur dioxide, nitrogen dioxide and nitric oxide, and in addition, tar particles, hydrocarbons, CO2, H2O, 3, 4-benzopyrene and the like.
The traditional flue gas treatment method mainly comprises a solid absorption method and a liquid absorption method; the solid absorption method is mainly used for solidifying sulfur through the reaction of magnesium oxide and the like and sulfur dioxide; the disadvantage is that the absorption rate is poor and the smoke components can not be effectively absorbed. Although the liquid absorption method has high absorption rate, high-temperature flue gas is collected from the top of the tower and introduced into liquid through a pipeline (generally adopting ammonia water for absorption); the flue gas has acid corrosion, so the requirement on equipment is high, the cost is very high, and generally small and medium-sized enterprises cannot support the higher cost, and the flue gas is not suitable for large-area popularization and application.
Therefore, the research on a solid adsorbent capable of effectively absorbing smoke pollutants is one of the important subjects studied by those skilled in the art.
Disclosure of Invention
The invention aims to solve the problems, provides a petroleum coke calcination waste gas adsorbent and a preparation method and application thereof, and realizes the following purposes: the sulfur dioxide, nitrogen dioxide, nitric oxide, tar particles, hydrocarbons and 3, 4-benzopyrene in the petroleum coke calcination waste gas are effectively absorbed, and the absorption rate of smoke pollutants is improved.
In order to realize the purpose of the invention, the following technical scheme is adopted:
the petroleum coke calcination waste gas adsorbent comprises the following components in parts by weight: 32-35 parts of activated carbon, 12-16 parts of coconut shell fiber, 4.5-5.6 parts of nano calcium carbonate, 5.7-6.2 parts of graphene, 1.2-1.8 parts of pentaerythritol, 0.6-0.9 part of delphinidin, 0.15-0.32 part of lutein, 2-3 parts of ethyl acetate, 1.2-1.6 parts of ammonium molybdate and 2.3-2.9 parts of sodium tripolyphosphate.
The active carbon is composed of coconut shell active carbon, sepiolite active carbon and apricot shell active carbon according to the mass ratio of 2:1: 3;
the coconut shell fiber: the fineness is 1.5-2dtex, the fiber length is 80-90 mu m, and the water content is 6-7%;
the nano calcium carbonate: calcium carbonate content not less than 99%, water content<0.3%, pH 9.0-10.0, and insoluble in hydrochloric acid<0.2% and a density of 2.7mg/cm3The fineness is 3000 meshes; the graphene: the fineness is 30-50 μm.
The preparation method comprises the following steps:
preparing raw materials: weighing the raw material components according to the formula proportion for later use.
Step 1, preparation of activated carbon
Mixing coconut shell activated carbon, sepiolite activated carbon and apricot shell activated carbon according to the mass ratio of 2:1:3, and grinding to 100 meshes to obtain activated carbon;
the activated carbon has the mesoporous rate of 95.4-95.8 percent, the moisture content of 4-5 percent, the ash content of 2.3-2.7 percent, the bulk density of 385-388g/L, the specific surface area of 1480-1520m2/g and the average pore diameter of 3.5-4.2 nm.
Step 2, activation
Mixing activated carbon with pentaerythritol, delphinidin, lutein and ethyl acetate, and making into dispersion with water, wherein the mass concentration of the dispersion is 42-45%; heating the dispersion to 60-65 ℃, and carrying out heat treatment for 5 hours; evaporating and dehydrating to obtain a primary activated material, and cooling to normal temperature.
Step 3, secondary activation
Uniformly mixing the primary activated material and a secondary activating agent, and activating for 40min at 160 ℃ under the protection of nitrogen with the flow of N2 of 40ml/min to obtain an activated material; the secondary activating agent is a mixture of ammonium molybdate and sodium tripolyphosphate, and the mass ratio of the ammonium molybdate to the sodium tripolyphosphate is 12-16: 23-29.
Step 4, preparing a finished product
Mixing the activated material prepared in the step 3 with coconut shell fibers, nano calcium carbonate and graphene; mixing at 1800rpm for 40-50min to obtain adsorbent product.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the absorbent has the absorption rate of 95.3-96.7% for sulfur dioxide, 89.3-94.3% for nitrogen dioxide, 99.4-99.5% for nitric oxide, 99.8-99.9% for tar particles, 99.8-99.9% for hydrocarbons and 100% for 3, 4-benzopyrene. Detailed Description
Example 1 absorbent for exhaust gas from calcination of Petroleum Coke
The petroleum coke calcination waste gas adsorbent comprises the following components: 32 parts of activated carbon, 16 parts of coconut shell fiber, 4.5 parts of nano calcium carbonate, 6.2 parts of graphene, 1.2 parts of pentaerythritol, 0.6 part of delphinidin, 0.32 part of lutein, 2 parts of ethyl acetate, 1.6 parts of ammonium molybdate and 2.9 parts of sodium tripolyphosphate.
The active carbon is composed of coconut shell active carbon, sepiolite active carbon and apricot shell active carbon according to the mass ratio of 2:1: 3;
the coconut shell fiber: fineness of 1.5dtex, fiber length of 90 μm, and water content of 7%;
the nano calcium carbonate: calcium carbonate content not less than 99%, water content<0.3%, pH 9.0-10.0, and insoluble in hydrochloric acid<0.2% and a density of 2.7mg/cm3The fineness is 3000 meshes; the graphene: the fineness was 30 μm.
The preparation method comprises the following steps:
preparing raw materials: weighing the raw material components according to the formula proportion for later use.
Step 1, preparation of activated carbon
Mixing coconut shell activated carbon, sepiolite activated carbon and apricot shell activated carbon according to the mass ratio of 2:1:3, and grinding to 100 meshes to obtain activated carbon;
the activated carbon has the advantages of 95.4 percent of mesoporous rate, 5 percent of moisture content, 2.7 percent of ash, 388g/L of bulk density, 1480m2/g of specific surface area and 4.2nm of average pore diameter.
Step 2, activation
Mixing activated carbon with pentaerythritol, delphinidin, lutein and ethyl acetate uniformly, and preparing a dispersion with water, wherein the mass concentration of the dispersion is 42%; heating the dispersion to 60 ℃, and carrying out heat treatment for 5 hours; evaporating and dehydrating to obtain a primary activated material, and cooling to normal temperature.
Step 3, secondary activation
Uniformly mixing the primary activated material and a secondary activating agent, and activating for 40min at 160 ℃ under the protection of nitrogen with the flow of N2 of 40ml/min to obtain an activated material; the secondary activating agent is a mixture of ammonium molybdate and sodium tripolyphosphate, and the mass ratio of the ammonium molybdate to the sodium tripolyphosphate is 16: 29.
Step 4, preparing a finished product
Mixing the activated material prepared in the step 3 with coconut shell fibers, nano calcium carbonate and graphene; mixing at 1800rpm for 40min to obtain adsorbent product.
Example 2 absorbent for exhaust gas from petroleum coke calcination
The petroleum coke calcination waste gas adsorbent comprises the following components: 33 parts of activated carbon, 14 parts of coconut shell fiber, 5.5 parts of nano calcium carbonate, 5.8 parts of graphene, 1.5 parts of pentaerythritol, 0.8 part of delphinidin, 0.25 part of lutein, 2.5 parts of ethyl acetate, 1.4 parts of ammonium molybdate and 2.6 parts of sodium tripolyphosphate.
The active carbon is composed of coconut shell active carbon, sepiolite active carbon and apricot shell active carbon according to the mass ratio of 2:1: 3;
the coconut shell fiber: the fineness was 2dtex, the fiber length was 85 μm, and the water content was 6.5%;
the nano calcium carbonate: calcium carbonate content not less than 99%, water content<0.3%, pH 9.0-10.0, and insoluble in hydrochloric acid<0.2% and a density of 2.7mg/cm3The fineness is 3000 meshes; the graphene: the fineness was 40 μm.
The preparation method comprises the following steps:
preparing raw materials: weighing the raw material components according to the formula proportion for later use.
Step 1, preparation of activated carbon
Mixing coconut shell activated carbon, sepiolite activated carbon and apricot shell activated carbon according to the mass ratio of 2:1:3, and grinding to 100 meshes to obtain activated carbon;
the activated carbon has the advantages of 95.8 percent of mesoporous rate, 4 percent of moisture content, 2.3 percent of ash, 385g/L of bulk density, 1520m2/g of specific surface area and 3.5nm of average pore diameter.
Step 2, activation
Uniformly mixing activated carbon with pentaerythritol, delphinidin, lutein and ethyl acetate, and preparing a dispersion liquid with water, wherein the mass concentration of the dispersion liquid is 45%; heating the dispersion to 65 ℃ and carrying out heat treatment for 5 hours; evaporating and dehydrating to obtain a primary activated material, and cooling to normal temperature.
Step 3, secondary activation
Uniformly mixing the primary activated material and a secondary activating agent, and activating for 40min at 160 ℃ under the protection of nitrogen with the flow of N2 of 40ml/min to obtain an activated material; the secondary activating agent is a mixture of ammonium molybdate and sodium tripolyphosphate, and the mass ratio of the ammonium molybdate to the sodium tripolyphosphate is 14: 26.
Step 4, preparing a finished product
Mixing the activated material prepared in the step 3 with coconut shell fibers, nano calcium carbonate and graphene; mixing at 1800rpm for 50min to obtain adsorbent product.
Example 3 absorbent for exhaust gas from Petroleum Coke calcination
The petroleum coke calcination waste gas adsorbent comprises the following components: 35 parts of activated carbon, 12 parts of coconut shell fiber, 5.6 parts of nano calcium carbonate, 5.7 parts of graphene, 1.8 parts of pentaerythritol, 0.9 part of delphinidin, 0.15 part of lutein, 3 parts of ethyl acetate, 1.2 parts of ammonium molybdate and 2.3 parts of sodium tripolyphosphate.
The active carbon is composed of coconut shell active carbon, sepiolite active carbon and apricot shell active carbon according to the mass ratio of 2:1: 3;
the coconut shell fiber: the fineness was 1.8dtex, the fiber length was 85 μm, and the water content was 6.6%;
the nano calcium carbonate: calcium carbonate content not less than 99%, water content<0.3%, pH 9.0-10.0, and insoluble in hydrochloric acid<0.2% and a density of 2.7mg/cm3The fineness is 3000 meshes; the graphene: the fineness was 50 μm.
The preparation method comprises the following steps:
preparing raw materials: weighing the raw material components according to the formula proportion for later use.
Step 1, preparation of activated carbon
Mixing coconut shell activated carbon, sepiolite activated carbon and apricot shell activated carbon according to the mass ratio of 2:1:3, and grinding to 100 meshes to obtain activated carbon;
the activated carbon has the advantages of 95.5 percent of mesoporous rate, 4.6 percent of moisture content, 2.6 percent of ash, 386g/L of bulk density, 1490m2/g of specific surface area and 3.9nm of average pore diameter.
Step 2, activation
Mixing activated carbon with pentaerythritol, delphinidin, lutein and ethyl acetate uniformly, and preparing a dispersion with water, wherein the mass concentration of the dispersion is 43%; heating the dispersion to 63 ℃ and carrying out heat treatment for 5 hours; evaporating and dehydrating to obtain a primary activated material, and cooling to normal temperature.
Step 3, secondary activation
Uniformly mixing the primary activated material and a secondary activating agent, and activating for 40min at 160 ℃ under the protection of nitrogen with the flow of N2 of 40ml/min to obtain an activated material; the secondary activating agent is a mixture of ammonium molybdate and sodium tripolyphosphate, and the mass ratio of the ammonium molybdate to the sodium tripolyphosphate is 12: 23.
Step 4, preparing a finished product
Mixing the activated material prepared in the step 3 with coconut shell fibers, nano calcium carbonate and graphene; mixing at 1800rpm for 45min to obtain adsorbent product.
Through tests, the adsorbent of the embodiment 1-3 is placed in a filler layer of a flue gas absorption device, the height of the filler layer is 50cm, and the flue gas absorption device is positioned at the exhaust outlet end of petroleum coke calcination; the flue gas generated by calcining the petroleum coke can smoothly enter the flue gas absorption device filled with the adsorbent. Detecting the content of pollutants in the flue gas which does not pass through the flue gas absorption device, wherein the pollutants contain 360 mu g/Nm of sulfur dioxide3487 ug/Nm of nitrogen dioxide3Nitric oxide 315. mu.g/Nm3110. mu.g/Nm of tar particles388. mu.g/Nm of hydrocarbons33, 4-benzopyrene 70 mu g/Nm3。
The content of pollutants in the exhaust gas after passing through the smoke absorption device is detected, and the detection results are shown in the following table:
as can be seen from the above table, the sulfur dioxide content after adsorption by the adsorbent of the present invention is 12-17. mu.g/Nm328-52 mu g/Nm of nitrogen dioxide31.6-1.9 mug/Nm of nitric oxide3Tar particles 0.08-0.17 μ g/Nm30.12-0.21. mu.g/Nm of hydrocarbons3And 3, 4-benzopyrene is 0, and pollutants in petroleum coke calcination waste gas are effectively absorbed.
The absorption rate of the adsorbent is 95.3-96.7% for sulfur dioxide, 89.3-94.3% for nitrogen dioxide, 99.4-99.5% for nitric oxide, 99.8-99.9% for tar particles, 99.8-99.9% for hydrocarbons and 100% for 3, 4-benzopyrene.
Except for special description, the percentages are mass percentages, and the ratios are mass ratios.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. The petroleum coke calcination waste gas adsorbent is characterized in that: the material comprises the following raw material components in parts by weight: 32-35 parts of activated carbon, 12-16 parts of coconut shell fiber, 4.5-5.6 parts of nano calcium carbonate, 5.7-6.2 parts of graphene, 1.2-1.8 parts of pentaerythritol, 0.6-0.9 part of delphinidin, 0.15-0.32 part of lutein, 2-3 parts of ethyl acetate, 1.2-1.6 parts of ammonium molybdate and 2.3-2.9 parts of sodium tripolyphosphate;
the active carbon is composed of coconut shell active carbon, sepiolite and apricot shell active carbon according to the mass ratio of 2:1: 3;
the coconut shell fiber: the titer is 1.5-2dtex, the fiber length is 80-90 μm, and the water content is 6-7%;
the nano calcium carbonate: calcium carbonate content not less than 99%, water content<0.3%, pH 9.0-10.0, hydrochloric acid insoluble substance<0.2% and a density of 2.7mg/cm3 The fineness is 3000 meshes; the graphene: the fineness is 30-50 μm;
the preparation method of the petroleum coke calcination waste gas adsorbent comprises the steps of preparation, activation and secondary activation of activated carbon;
the preparation of the activated carbon comprises the following steps: the coconut shell activated carbon sepiolite and apricot shell activated carbon are mixed according to the mass ratio of 2:1:3 to prepare the coconut shell activated carbon nano composite material; the prepared active carbon has the mesoporous rate of 95.4-95.8 percent, the water content of 4-5 percent, the ash content of 2.3-2.7 percent and the bulk density of 385-1480-1520m specific surface area2 (ii)/g, average pore diameter is 3.5-4.2 nm;
the activation: mixing activated carbon with pentaerythritol, delphinidin, lutein and ethyl acetate, and making into dispersion with water, wherein the mass concentration of the dispersion is 42-45%; heating the dispersion liquid to 60-65 ℃, and carrying out heat treatment for 5 hours to obtain a primary activated material;
and (3) secondary activation: uniformly mixing the primary activating material and the secondary activating agent, and then adding N2 Activating for 40min at 160 ℃ under the protection of nitrogen with the flow of 40ml/min to obtain an activated material; the secondary activating agent is a mixture of ammonium molybdate and sodium tripolyphosphate, and the mass ratio of the ammonium molybdate to the sodium tripolyphosphate is 12-16: 23-29.
2. The use of the petroleum coke calcination waste gas adsorbent according to claim 1, wherein: the application is as follows: the adsorbent is placed in a packing layer of a flue gas absorption device, the height of the packing layer is 50cm, and the flue gas absorption device is positioned at a petroleum coke calcination exhaust outlet end; the flue gas generated by calcining the petroleum coke can smoothly enter the flue gas absorption device filled with the adsorbent.
3. The use of the petroleum coke calcination waste gas adsorbent according to claim 2, wherein: the absorption rate of the adsorbent to sulfur dioxide in the waste gas is 95.3-96.7%, the absorption rate to nitrogen dioxide in the waste gas is 89.3-94.3%, and the absorption rate to nitric oxide in the waste gas is 99.4-99.5%.
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| CN111762869B (en) * | 2020-06-23 | 2022-06-28 | 生态环境部南京环境科学研究所 | Sewage treatment plant based on modified activated carbon biological filter |
| CN112774388A (en) * | 2021-02-04 | 2021-05-11 | 钟学能 | Waste gas treatment device for tobacco drying and use method thereof |
| CN114558441B (en) * | 2022-03-02 | 2023-05-30 | 通化鑫鸿新材料有限公司 | Preparation method and application of solid high-fluidity, high-efficiency and low-byproduct nano calcium carbonate denitration agent |
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| 石油焦煅烧烟气脱硫技术分析;吕阳华;《化工管理》;20180430;第128-129页 * |
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