CN104194808A - Method for catalytic pyrolysis of rice hulls - Google Patents
Method for catalytic pyrolysis of rice hulls Download PDFInfo
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- CN104194808A CN104194808A CN201410391217.XA CN201410391217A CN104194808A CN 104194808 A CN104194808 A CN 104194808A CN 201410391217 A CN201410391217 A CN 201410391217A CN 104194808 A CN104194808 A CN 104194808A
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- rice husk
- iron oxide
- oxide powder
- catalytic pyrolysis
- pyrolysis
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- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 56
- 235000009566 rice Nutrition 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000007233 catalytic pyrolysis Methods 0.000 title claims abstract description 14
- 240000007594 Oryza sativa Species 0.000 title 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 241000209094 Oryza Species 0.000 claims abstract description 55
- 239000000843 powder Substances 0.000 claims abstract description 22
- 230000004580 weight loss Effects 0.000 claims abstract description 18
- 230000004913 activation Effects 0.000 claims abstract description 12
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 12
- 239000010903 husk Substances 0.000 claims description 51
- 238000000197 pyrolysis Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 9
- 238000002474 experimental method Methods 0.000 claims description 6
- 238000011160 research Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000002028 Biomass Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Processing Of Solid Wastes (AREA)
Abstract
Description
技术领域technical field
本发明涉及一种用于稻壳催化热解的方法，属于能源技术领域。The invention relates to a method for catalytic pyrolysis of rice husk, which belongs to the technical field of energy.
背景技术Background technique
稻壳是重要的农业废弃物之一，仅中国每年就有约4000万吨的产量。作为一种可再生的生物质资源，稻壳通常用作燃料直接燃烧以提供热量，但利用品位相对较低。热解是目前生物质研究的热点技术之一，通过热解，可以将稻壳转化为高品位的可燃气和易存储、运输且能量密度高的焦油，以及工业上需求量很大的活性炭和具有高附加值的无定形二氧化硅。Rice husk is one of the important agricultural wastes, with an annual output of about 40 million tons in China alone. As a renewable biomass resource, rice husk is usually burned directly as fuel to provide heat, but the utilization grade is relatively low. Pyrolysis is one of the hot technologies in biomass research at present. Through pyrolysis, rice husk can be converted into high-grade combustible gas and tar which is easy to store and transport and has high energy density, as well as activated carbon and Amorphous silica with high added value.
热解是指在没有含氧气体介质参与的情况下，单纯利用热使生物质中的有机物发生分解从而脱除挥发性物质，并形成固态半焦或焦炭的过程。热解产物包括气体、液体和固体三种，其中气体可直接用作燃料；液体可通过进一步分离和提取制成燃料油和化工原料；固体可用作化工生产所需的活性炭等。Pyrolysis refers to the process of decomposing organic matter in biomass by simply using heat without the participation of an oxygen-containing gas medium to remove volatile substances and form solid semi-coke or coke. Pyrolysis products include gas, liquid and solid. Gas can be used directly as fuel; liquid can be further separated and extracted to make fuel oil and chemical raw materials; solid can be used as activated carbon for chemical production.
反应温度、升温速率和气体停留时间等外部条件以及生物质化学组分、粒径大小和导热性能等内部条件都会对生物质热解特性以及各相产物的最终产率、组分和比重产生影响，我国目前已基本掌握稻壳热解的基本特性，但对于如何提高热解程度的研究还相对较少，因此制备具有催化热解作用的催化剂是热解研究的重点。External conditions such as reaction temperature, heating rate, and gas residence time, as well as internal conditions such as biomass chemical composition, particle size, and thermal conductivity, will affect the pyrolysis characteristics of biomass and the final yield, composition, and specific gravity of each phase product. At present, my country has basically mastered the basic characteristics of rice husk pyrolysis, but there are relatively few studies on how to improve the degree of pyrolysis. Therefore, the preparation of catalysts with catalytic pyrolysis is the focus of pyrolysis research.
发明内容Contents of the invention
本发明的目的在于提供一种用于稻壳催化热解的方法。选取武运粳7号稻壳作为实验原料，通过添加氧化铁粉末作为催化剂，计算其催化前后失重率(DT)、失重速率(DTG)以及活化能变化，实验结果表明，稻壳在氧化铁的催化作用下能够热解的更加彻底，活化能减小了10％左右，更加有利于稻壳的充分利用。The purpose of the present invention is to provide a method for catalytic pyrolysis of rice husk. The rice husk of Wuyunjing No. 7 was selected as the experimental raw material, and the weight loss rate (DT), weight loss rate (DTG) and activation energy changes before and after the catalysis were calculated by adding iron oxide powder as the catalyst. Under the action of catalysis, it can be pyrolyzed more thoroughly, and the activation energy is reduced by about 10%, which is more conducive to the full utilization of rice husks.
实现本发明的技术方案为：Realize the technical scheme of the present invention as:
一种用于催化稻壳热解的新应用，所述催化剂为氧化铁粉末，粒径为≥100目。实验材料为武运粳7号稻壳，利用粉碎机将其粉碎成粒径≤1mm，在105℃下干燥24h。实验在恒久差热天平下进行。A new application for catalyzing the pyrolysis of rice husk, the catalyst is iron oxide powder with a particle size of ≥100 mesh. The experimental material is Wuyunjing No. 7 rice husk, which is crushed into a particle size of ≤1mm by a pulverizer, and dried at 105°C for 24 hours. The experiments were carried out under a permanent differential thermobalance.
本发明中过加入氧化铁粉末用于稻壳的催化热解，具体步骤如下：Among the present invention, adding iron oxide powder is used for the catalytic pyrolysis of rice husk, and concrete steps are as follows:
1)将稻壳粉碎，并在干燥箱中干燥得到干燥基，同时筛选出氧化铁粉末；1) The rice husk is pulverized, and dried in a drying oven to obtain a dry base, while screening out iron oxide powder;
2)将稻壳和氧化铁粉末混合，并搅拌；2) rice husk and iron oxide powder are mixed and stirred;
3)分别对催化前后的稻壳进行热解实验研究，并对实验数据进行分析。3) Conduct pyrolysis experiments on rice husks before and after catalysis, and analyze the experimental data.
步骤1)中，稻壳粉碎粒径为≤1mm，干燥温度为95-105℃，干燥时间为16-24h；氧化铁粉末粒径≥100目。In step 1), the particle size of the crushed rice husk is ≤1 mm, the drying temperature is 95-105° C., and the drying time is 16-24 hours; the particle size of the iron oxide powder is ≥100 mesh.
步骤2)中，氧化铁粉末的质量占稻壳质量的10％-20％。In step 2), the mass of iron oxide powder accounts for 10%-20% of the mass of rice husk.
步骤3)中，实验研究方法为非等温法，即分别以5℃/min、10℃/min、15℃/min、20℃/min加热样品到700-1000℃；计算催化前后失重率、失重速率以及活化能变化。实验结果分析方法为Coats-Redfern法。In step 3), the experimental research method is a non-isothermal method, that is, heating the sample to 700-1000°C at 5°C/min, 10°C/min, 15°C/min, and 20°C/min respectively; calculating the weight loss rate before and after catalysis, weight loss rate and activation energy changes. The analysis method of the experimental results is the Coats-Redfern method.
本发明与现有技术相比，其显著优点是：Compared with the prior art, the present invention has the remarkable advantages of:
(1)氧化铁作为催化剂较为廉价，从而催化成本较低。(1) Iron oxide is relatively cheap as a catalyst, so the catalytic cost is relatively low.
(2)氧化铁容易获得，无需加工处理，简化催化步骤。(2) Iron oxide is easy to obtain, no processing is required, and the catalytic steps are simplified.
(3)与常规的碱金属催化相比，氧化铁较为稳定，适合多次循环利用。(3) Compared with conventional alkali metal catalysis, iron oxide is more stable and suitable for multiple recycling.
附图说明Description of drawings
图1稻壳热解TG曲线。Fig. 1 TG curve of rice husk pyrolysis.
图2稻壳催化热解TG曲线。Fig. 2 TG curve of catalytic pyrolysis of rice husk.
图3稻壳的ln[G(α)/T2]-1/RT线性关系图。Fig. 3 The linear relationship diagram of ln[G(α)/T 2 ]-1/RT of rice husk.
图4稻壳催化的ln[G(α)/T2]-1/RT线性关系图。Fig. 4 The linear relationship diagram of ln[G(α)/T 2 ]-1/RT catalyzed by rice husk.
具体实施方式Detailed ways
一种用于催化稻壳热解的新应用，所述催化剂为氧化铁粉末，粒径为≥100目。实验材料为武运粳7号稻壳，利用粉碎机将其粉碎成粒径≤1mm，在105℃下干燥24h。实验在恒久差热天平下进行。A new application for catalyzing the pyrolysis of rice husk, the catalyst is iron oxide powder with a particle size of ≥100 mesh. The experimental material is Wuyunjing No. 7 rice husk, which is crushed into a particle size of ≤1mm by a pulverizer, and dried at 105°C for 24 hours. The experiments were carried out under a permanent differential thermobalance.
本发明中过加入氧化铁粉末用于稻壳的催化热解，具体步骤如下：Among the present invention, adding iron oxide powder is used for the catalytic pyrolysis of rice husk, and concrete steps are as follows:
1)将稻壳粉碎，并在干燥箱中干燥得到干燥基，同时筛选出氧化铁粉末；1) The rice husk is pulverized, and dried in a drying oven to obtain a dry base, while screening out iron oxide powder;
2)将稻壳和氧化铁粉末混合，并搅拌；2) rice husk and iron oxide powder are mixed and stirred;
3)分别对催化前后的稻壳进行热解实验研究，并对实验数据进行分析。3) Conduct pyrolysis experiments on rice husks before and after catalysis, and analyze the experimental data.
步骤1)中，稻壳粉碎粒径为≤1mm，干燥温度为95-105℃，干燥时间为16-24h；氧化铁粉末粒径≥100目。In step 1), the particle size of the crushed rice husk is ≤1 mm, the drying temperature is 95-105° C., and the drying time is 16-24 hours; the particle size of the iron oxide powder is ≥100 mesh.
步骤2)中，氧化铁粉末的质量占稻壳质量的10％-20％。In step 2), the mass of iron oxide powder accounts for 10%-20% of the mass of rice husk.
步骤3)中，实验研究方法为非等温法，即分别以5℃/min、10℃/min、15℃/min、20℃/min加热样品到700-1000℃；计算催化前后失重率、失重速率以及活化能变化。实验结果分析方法为Coats-Redfern法。In step 3), the experimental research method is a non-isothermal method, that is, heating the sample to 700-1000°C at 5°C/min, 10°C/min, 15°C/min, and 20°C/min respectively; calculating the weight loss rate before and after catalysis, weight loss rate and activation energy changes. The analysis method of the experimental results is the Coats-Redfern method.
下面结合附图和实施例对本发明作进一步详细描述。The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments.
实施例1Example 1
制取粒径≤1mm的稻壳，在105℃下进行干燥，干燥时间为24h，称取5.0mg稻壳和1mg氧化铁粉末，充分混合后加入差热天平中，利用非等温法分别以5℃/min、10℃/min、15℃/min、20℃/min加热样品到1000℃，得到失重曲线，并分别求出失重曲线曲线，如图1和图2。Prepare rice husks with a particle size of ≤1 mm, dry them at 105°C for 24 hours, weigh 5.0 mg of rice husks and 1 mg of iron oxide powder, mix them thoroughly and add them to a differential thermal balance. ℃/min, 10℃/min, 15℃/min, 20℃/min heat the sample to 1000℃, obtain the weight loss curve, and calculate the weight loss curve respectively, as shown in Figure 1 and Figure 2.
通过两图比较可知，当温度达到390℃时，纯稻壳的失重约在60％-65％左右，而加氧化铁催化的稻壳的失重约在53％-58％左右，实验说明加氧化铁能够使稻壳热解更加彻底。From the comparison of the two figures, it can be seen that when the temperature reaches 390°C, the weight loss of pure rice husk is about 60%-65%, while the weight loss of rice husk catalyzed by iron oxide is about 53%-58%. Iron can make rice husk pyrolysis more thorough.
利用Coats-Redfern法计算催化前后的活化能，其积分形式为ln[G(α)/T2]＝ln[(AR)/(ΒE)]-E/(RT),做出ln[G(α)/T2]-1/RT关系曲线，如图3和图4，其斜率即为活化能E。Utilize the Coats-Redfern method to calculate the activation energy before and after catalysis, and its integral form is ln[G(α)/ T ]=ln[(AR)/(ΒE)]-E/(RT), make ln[G( α)/T 2 ]-1/RT relationship curve, as shown in Figure 3 and Figure 4, the slope is the activation energy E.
根据计算得出，稻壳热解的活化能117.47KJ/mol，加氧化铁催化的稻壳热解的活化能为104.97KJ/mol。实验得出通过加入氧化铁的催化，使得稻壳热解的活化能降低了10％左右，使反应更加容易发生，有利于工业上的大规模生产。According to the calculation, the activation energy of rice husk pyrolysis is 117.47KJ/mol, and the activation energy of rice husk pyrolysis catalyzed by adding iron oxide is 104.97KJ/mol. Experiments show that the activation energy of rice husk pyrolysis is reduced by about 10% by adding iron oxide as catalysis, which makes the reaction easier to occur and is beneficial to large-scale industrial production.
实施例2Example 2
制取粒径≤1mm的稻壳，在95℃下进行干燥，干燥时间为16h，称取5.0mg稻壳和2mg氧化铁粉末，充分混合后加入差热天平中，利用非等温法分别以5℃/min、10℃/min、15℃/min、20℃/min加热样品到800℃，得到失重曲线，并分别求出失重曲线曲线。Prepare rice husks with a particle size of ≤1 mm and dry them at 95°C for 16 hours. Weigh 5.0 mg of rice husks and 2 mg of iron oxide powder, mix them thoroughly and add them to a differential thermal balance. ℃/min, 10℃/min, 15℃/min, 20℃/min heat the sample to 800℃, obtain the weight loss curve, and calculate the weight loss curve respectively.
实施例3Example 3
制取粒径≤1mm的稻壳，在100℃下进行干燥，干燥时间为20h，称取5.0mg稻壳和1.5mg氧化铁粉末，充分混合后加入差热天平中，利用非等温法分别以5℃/min、10℃/min、15℃/min、20℃/min加热样品到900℃，得到失重曲线，并分别求出失重曲线曲线。Prepare rice husks with a particle size of ≤1 mm and dry them at 100°C for 20 hours. Weigh 5.0 mg of rice husks and 1.5 mg of iron oxide powder, mix them thoroughly and add them to a differential thermal balance. Heat the sample at 5°C/min, 10°C/min, 15°C/min, 20°C/min to 900°C, obtain the weight loss curve, and calculate the weight loss curve respectively.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104680003A (en) * | 2015-02-11 | 2015-06-03 | 中原工学院 | Prediction method for hydrothermal coke yield |
| CN105419829A (en) * | 2015-10-09 | 2016-03-23 | 青海威德生物技术有限公司 | Method for preparing biomass gas by pyrolyzing chicory residues |
| CN109097077A (en) * | 2018-10-19 | 2018-12-28 | 上海理工大学 | A kind of method of CO yield in reduction catalytic pyrolysis of biomass |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104680003A (en) * | 2015-02-11 | 2015-06-03 | 中原工学院 | Prediction method for hydrothermal coke yield |
| CN104680003B (en) * | 2015-02-11 | 2017-07-14 | 中原工学院 | A kind of Forecasting Methodology of hydro-thermal coke yield |
| CN105419829A (en) * | 2015-10-09 | 2016-03-23 | 青海威德生物技术有限公司 | Method for preparing biomass gas by pyrolyzing chicory residues |
| CN105419829B (en) * | 2015-10-09 | 2018-05-11 | 青海威德生物技术有限公司 | A kind of method for being pyrolyzed witloof residue and preparing biogas |
| CN109097077A (en) * | 2018-10-19 | 2018-12-28 | 上海理工大学 | A kind of method of CO yield in reduction catalytic pyrolysis of biomass |
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Application publication date: 20141210 |