CN101396660A - Biomass gasification tar cracking composite catalyst and preparation method thereof - Google Patents
Biomass gasification tar cracking composite catalyst and preparation method thereof Download PDFInfo
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- CN101396660A CN101396660A CNA2008101559718A CN200810155971A CN101396660A CN 101396660 A CN101396660 A CN 101396660A CN A2008101559718 A CNA2008101559718 A CN A2008101559718A CN 200810155971 A CN200810155971 A CN 200810155971A CN 101396660 A CN101396660 A CN 101396660A
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Abstract
The invention provides a preparation method of a biomass gasified tar cracking composite catalyst, comprising the following steps: first, the preparation of a binder: Ni(NO3)2.6H2O crystal and Al2O3 powder are weighed, the Al2O3 powder is added in the water solution of the Ni(NO3)2.6H2O crystal, immersed for 2h-4h at constant temperature water bath of 40 DEG C, dried into light green powder and calcinated; second, the pretreatment of dolomite: the dolomite is ground into powder of 200 meshes below; third, the preparation of a carrier of the composite catalyst: Fe2O3 and the dolomite powder are mixed uniformly and are added with the binder and 5-20mL of nitric acid to be mixed +-<*> uniformly, and the mixture is extruded to be molded, dried naturally, dried at 105 DGE C, calcinated under 400 DEG C and then calcinated at 900 DEG C; forth, the solution immersion of active components: Ni(NO3)2 ethanol solution is used for immersing the carrier of the composite catalyst, and after dried, the carrier is calcinated at 600-800 DGE C. the composite catalyst has the advantages of high catalytic activity, good strength, practical application and simple process.
Description
Technical field
The present invention relates to the Biomass Energy Utilization field, relate in particular to biomass gasification tar cracking Preparation of catalysts method.
Background technology
Biomass resource is unique reproducible carbon resource, can change into conventional liquid state and fuel gas and other industrial chemicals or product.Because of characteristics such as its aboundresources, renewable and environmental friendliness, be subject to people's attention.Biomass and Gasification Technology and exploitation are the importances of biomass energy transformation technology, also are that clean and effective utilizes one of effective way of biomass energy.
Living beings mainly produce CO, H in the pyrolytic gasification process
2, CO
2, CH
4, H
2O and N
2Deng gas, wherein also have organic and inorganic impurity of part and particle.The organic matter that produces in the biomass gasification process comprises little molecular carbon hydrogen compound and big molecule polynuclear aromatic family hydrocarbon (tar), is difficult to be applied directly in the follow-up workshop section.The existence of tar causes aerogenesis and energy loss, etching apparatus simultaneously, and blocking pipe has directly affected the application and development of biogas.From the present coercibility organic matter technology of removing, washing exists energy dissipation and secondary pollution phenomenon except coercibility organic matter method, and clean-up effect can only reach the requirement of internal combustion engine reluctantly; Pyrolysis method can obtain higher conversion efficiency more than 1100 ℃, but realizes difficulty in the practical application; Catalystic pyrolysis can be converted into combustible gas with tar, has both improved system's energy utilization rate, thoroughly reduces again secondary pollution, is present more rising technology.
Utilizing catalyst that tar is carried out catalytic pyrolysis is to reduce tar content, improves a kind of effective method of gasification efficiency.More to the research of catalytic pyrolysis both at home and abroad, research to living beings gasification generation tar at present mainly concentrates on the choosing of catalyst, in the experimentation, choose the lysis efficiency that correct catalyst can not only improve tar, obtain how useful gas, and can reach the purpose that reduces cost.Used catalyst mainly contains natural crystal class catalyst, alkali metal class catalyst and nickel-base catalyst.But the tar in certain single catalyst catalytic pyrolysis biological flue gas of simple dependence, effect is not ideal.So must prepare the superimposed composite catalyst of various active component, make each catalytic active substance performance effect the most efficiently.Because China's dolomite output is more, low price is that the research of tar cracking catalyst of carrier is more at present with the dolomite, so the composite catalyst in this patent is carrier with the dolomite, has suitably added the oxide of active component Fe and Ni.
In the research process of present biomass gasification tar cracking, it is imperative to develop safe, efficient and eco-friendly composite catalyst.Composite catalyst has advantages such as catalytic efficiency height, intensity is big, practical application technology is simple.Advanced person's catalyst preparation technology is applied to gasification of biomass and generation technology, effectively raises the gasification of biomass application level.
Summary of the invention
The invention provides the preparation method of the biomass coke tar catalyst for cracking that a kind of intensity is good, goudron lysis rate is high.
Technical scheme of the present invention is: a kind of preparation method of biomass gasification tar cracking composite catalyst comprises the steps:
The first step, the preparation of binding agent: Ni:Al in mass ratio
2O
3The ratio of=10～15:100 takes by weighing Ni (NO
3)
26H
2O crystal and Al
2O
3Powder is with Al
2O
3Powder adds Ni (NO
3)
26H
2In the aqueous solution of O crystal, in 40 ℃ of water-baths of constant temperature, flood 2h～4h, dry in 105 ℃ of insulating boxs, make the light green powder, again at 700 ℃ of lower roasting 2h～4h;
Second step, dolomite preliminary treatment: dolomite dust is broken into powder below 200 orders;
The 3rd step, the preparation of composite catalyzing agent carrier: with Fe
2O
3With in the second step through pretreated dolomite powder Fe in mass ratio
2O
3: the ratio of dolomite=5～10:95 mixes, and adds to account for Fe
2O
38%～15% the binding agent of being made by the first step with the dolomite gross mass adds concentration again at the nitric acid of 5～20mL of 5%～15%wt, mixes, extrusion modling, after the air dry, 105 ℃ of lower dry 20h～48h, at 400 ℃ of calcining 1h～2h, be warming up to 900 ℃ of calcining 4h～6h again;
The 4th step, active component solution dipping: with the Ni (NO of ethanol configuration 0.8～1.2mol/L
3)
2Solution, the composite catalyzing agent carrier that dipping obtained in the 3rd step under 0.5～1 atmospheric pressure is 60～105 ℃ of lower dry 5h～10h in temperature, and then at 600～800 ℃ of roasting 6h～8h.The 4th step can repeat 2～3 times to improve the active component content in the carrier.
The composite catalyst that the preparation method of described biomass gasification tar cracking composite catalyst makes, take the dolomite of the bigger extrusion modling of surface area as carrier, active component is nickel oxide and compound Fe oxide, and wherein the mass percent of nickel oxide is 5%～12%, Fe
2O
3Mass percent be 4%～10%.Because the Ni (NO of load
3)
2With the Ni (NO in the binding agent
3)
2The nickel oxide that generates after high-temperature calcination has two kinds, and these two kinds of oxides all belong to the active component of catalyst, so these two kinds of active materials are referred to as the oxide of nickel herein.
Beneficial effect: the tar that adopts the small stationary bed biomass gasifying directly to produce is estimated the composite catalyst activity, discovery is than the tar cracking catalyst of one matter, as dolime, commercial nickel-base catalyst etc., the composite catalyst that the present invention prepares possesses following advantage: the catalytic activity height, intensity is good, practical application technology is simple.Under identical strength detection method, dolomite is about 75% in intensity after the calcining, and the intensity of composite catalyst of the present invention can reach more than 90%.Adopt composite catalyst tar conversion ratio of the present invention to reach more than 99%.
The specific embodiment
Raw material adopts the natural mineral products-dolomite of Shangluo City, Shaanxi Province.The method of testing of impregnation rate adopts Liu Jinxiang. the research method chapter 3 heat of solid catalyst analyze application in catalyticing research (on) [J]. petrochemical industry, 2000,29 (5): P380 among the 378-391., " 2.2 reducing process determine that catalyst form " are measured.
Embodiment 1
(1) preparation of binding agent: Ni:Al in mass ratio
2O
3The ratio of=10:100 takes by weighing the Ni (NO of 4.96g
3)
26H
2The O crystal is dissolved in the distilled water of 4mL, adds the Al of 10g
2O
3Powder floods 2h in 40 ℃ of water-baths of constant temperature, dry in 105 ℃ of insulating boxs, makes the light green powder, again at 700 ℃ of lower roasting 2h;
(2) dolomite preliminary treatment: dolomite dust is broken into powder below 200 orders;
(3) preparation of composite catalyzing agent carrier: with Fe
2O
3With dolomite powder in the step (2) Fe in mass ratio
2O
3: the ratio of dolomite=10:95 takes by weighing Fe
2O
3Powder 8.6g, dolomite powder 81.4g mixes, and adds the binding agent that 9g step (1) is made, add again mass concentration and be the nitric acid of 5% 18mL, mix, extrusion modling is after the air dry, 105 ℃ of lower dry 20h, put into Muffle furnace again and slowly heat up, 400 ℃ of calcining 1h are warming up to 900 ℃ of calcining 4h;
(4) active component solution dipping: with the Ni (NO of ethanol configuration 1mol/L
3)
2Solution, the composite catalyzing agent carrier that obtains in the impregnation steps under 1 atmospheric pressure (3) is at 60 ℃ of lower dry 8h, then 600 ℃ of roasting 6h in Muffle furnace;
(5) step (4) twice repeatedly, the impregnation rate of last nickel oxide reaches 5.4%.
Embodiment 2
(1) preparation of binding agent: be Ni:Al in mass ratio
2O
3The ratio of=15:100 takes by weighing the Ni (NO of 7.43g
3)
26H
2The O crystal is dissolved in the distilled water of 5mL, adds the Al of 10g
2O
3Powder floods 4h in 40 ℃ of water-baths of constant temperature, dry in 105 ℃ of insulating boxs, makes the light green powder, again at 700 ℃ of lower roasting 4h;
(2) dolomite preliminary treatment: dolomite dust is broken into powder below 200 orders;
(3) preparation of composite catalyzing agent carrier: with Fe
2O
3With dolomite powder in the step (2) Fe in mass ratio
2O
3: the ratio of dolomite=5:95 takes by weighing Fe
2O
3Powder 4.5g, dolomite powder 85.5g mixes, and adds the binding agent that 9g step (1) is made, add again 5mL concentration and be 15% nitric acid, mix, extrusion modling is after the air dry, 105 ℃ of lower dry 24h, put into Muffle furnace again and slowly heat up, 400 ℃ of calcining 2h are warming up to 900 ℃ of calcining 6h;
(4) active component solution dipping: with the Ni (NO of ethanol configuration 0.8mol/L
3)
2Solution, the composite catalyzing agent carrier that obtains in the impregnation steps (3) under 0.5 atmospheric pressure is at 105 ℃ of lower dry 5h, then 800 ℃ of roasting 6h in Muffle furnace;
(5) step (4) three times repeatedly, the impregnation rate of last nickel oxide reaches 6.7%.
The tar that adopts the small stationary bed biomass gasifying directly to produce is estimated the composite catalyst activity.
Earlier with V (H
2): V (N
2The reducing gases of)=5:95 is warmed up to 750 ℃, is connected with the fixed bed biomass gasification system behind the reductase 12 h, owing to adopt the form of fixed bed, in the entire reaction course, adopting flow is the N of 10mL/min
2The gas biological flue gas that produces is brought in the gas-chromatography test compound activity of such catalysts.Reaction end gas Tianjin, island 2014 type gas-chromatography on-line analyses of transforming, N
2, CO, CO
2, CH
4, H
2Adopt TCD to detect, tar adopts the GC-MS off-line analysis.
Embodiment 1 evaluating catalyst result is as shown in table 1:
| The material title | Catalyst-free | Embodiment 1 composite catalyst |
| H 2 | 0.43 | 1.43 |
| CO | 0.04 | 0.34 |
| CH 4 | 0.12 | 0.16 |
| CO 2 | 0.74 | 2.63 |
| Tar content (mg) | 252.4 | 2.1 |
| Tar conversion ratio (%) | 0 | 99.17 |
Embodiment 2 evaluating catalyst results are as shown in table 2:
| The material title | Catalyst-free | Embodiment 2 composite catalysts |
| H 2 | 0.43 | 2.36 |
| CO | 0.04 | 1.21 |
| CH 4 | 0.12 | 0.29 |
| CO 2 | 0.74 | 1.93 |
| Tar content (mg) | 252.4 | 1.2 |
| Tar conversion ratio (%) | 0 | 99.52 |
Embodiment 3
(1) preparation of binding agent: be Ni:Al in mass ratio
2O
3The ratio of=12:100 takes by weighing Ni (NO
3)
26H
2The O crystal is dissolved in the distilled water, adds Al
2O
3Powder floods 3h in 40 ℃ of water-baths of constant temperature, dry in 105 ℃ of insulating boxs, makes the light green powder, again at 700 ℃ of lower roasting 3h;
(2) dolomite preliminary treatment: dolomite dust is broken into powder below 200 orders;
(3) preparation of composite catalyzing agent carrier: with Fe
2O
3With dolomite powder in the step (2) Fe in mass ratio
2O
3: the ratio of dolomite=5:95 takes by weighing Fe
2O
3Powder and dolomite powder mix, and add to account for Fe
2O
3With the binding agent that 12% step (1) of dolomite gross mass is made, add again 20mL concentration and be 12% nitric acid, mix, extrusion modling, after the air dry, 105 ℃ of lower dry 34h, put into Muffle furnace again and slowly heat up, 400 ℃ of calcining 1.5h are warming up to 900 ℃ of calcining 5h;
(4) active component solution dipping: with the Ni (NO of ethanol configuration 1.2mol/L
3)
2Solution, the composite catalyzing agent carrier that obtains in the impregnation steps (3) under 0.7 atmospheric pressure is at 105 ℃ of lower dry 8h, then 800 ℃ of roasting 7h in Muffle furnace;
(5) step (4) three times repeatedly, the impregnation rate of last nickel oxide reaches 12.0%.
Claims (3)
1, a kind of preparation method of biomass gasification tar cracking composite catalyst is characterized in that comprising the steps:
The first step, the preparation of binding agent: Ni:Al in mass ratio
2O
3The ratio of=10～15:100 takes by weighing Ni (NO
3)
26H
2O crystal and Al
2O
3Powder is with Al
2O
3Powder adds Ni (NO
3)
26H
2In the aqueous solution of O crystal, in 40 ℃ of water-baths of constant temperature, flood 2h～4h, dry in 105 ℃ of insulating boxs, make the light green powder, again at 700 ℃ of lower roasting 2h～4h;
Second step, dolomite preliminary treatment: dolomite dust is broken into powder below 200 orders;
The 3rd step, the preparation of composite catalyzing agent carrier: with Fe
2O
3With in the second step through pretreated dolomite powder Fe in mass ratio
2O
3: the ratio of dolomite=5～10:95 mixes, and adds to account for Fe
2O
38%～15% the binding agent of being made by the first step with the dolomite gross mass adds concentration again at the nitric acid of 5%～15%wt5～20mL, mixes, extrusion modling, after the air dry, 105 ℃ of lower dry 20h～48h, at 400 ℃ of calcining 1h～2h, be warming up to 900 ℃ of calcining 4h～6h again;
The 4th step, active component solution dipping: with the Ni (NO of ethanol configuration 0.8～1.2mol/L
3)
2Solution, the composite catalyzing agent carrier that dipping obtained in the 3rd step under 0.5～1 atmospheric pressure is 60～105 ℃ of lower dry 5h～10h in temperature, and then at 600～800 ℃ of roasting 6h～8h.
2. the preparation method of biomass gasification tar cracking composite catalyst as claimed in claim 1 is characterized in that the 4th step repeated 2～3 times.
3. the composite catalyst that makes of the preparation method of biomass gasification tar cracking composite catalyst as claimed in claim 1, it is characterized in that described composite catalyst is take dolomite as carrier, active component is nickel oxide and compound Fe oxide, wherein the mass percent of nickel oxide is 5%～12%, Fe
2O
3Mass percent be 4%～10%.
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|---|---|---|---|
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|---|---|---|---|
| CN2008101559718A CN101396660B (en) | 2008-10-22 | 2008-10-22 | Biomass gasification tar cracking composite catalyst and preparation method thereof |
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|---|---|
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| CN101396660B CN101396660B (en) | 2010-08-25 |
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|---|---|---|---|
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| CN102059122A (en) * | 2010-11-15 | 2011-05-18 | 苏忠 | Catalyst for splitting oil tar and preparation method thereof |
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| CN101975406A (en) * | 2010-11-08 | 2011-02-16 | 张新才 | Nickel-based catalyst biomass gasification furnace |
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| CN102179247A (en) * | 2011-03-21 | 2011-09-14 | 上海大学 | Method for preparing hollow spherical nickel-based catalyst for catalytic pyrolysis of oil tar |
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| CN105312056A (en) * | 2014-06-26 | 2016-02-10 | Sk新技术株式会社 | Catalysts based on natural minerals and process for gasification using the same |
| CN104549450A (en) * | 2015-01-14 | 2015-04-29 | 天津大学 | Method for preparing loaded molecular sieve catalyst by using catalytic cracking of biomass gasification tar |
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| CN106563453A (en) * | 2016-10-27 | 2017-04-19 | 中国林业科学研究院林产化学工业研究所 | Composite catalyst for biomass gasification for preparing hydrogen-rich combustion gas, and preparation method thereof |
| CN106732704A (en) * | 2016-11-22 | 2017-05-31 | 新奥生态环境治理有限公司 | A kind of antigravity system for reducing biomass char oil content in bio oil |
| CN106732704B (en) * | 2016-11-22 | 2019-08-06 | 新奥生态环境治理有限公司 | A kind of antigravity system reducing biomass char oil content in bio oil |
| CN108970616A (en) * | 2017-05-30 | 2018-12-11 | 镇江杜微人才咨询有限公司 | A kind of preparation method of biomass tar cracking catalyst |
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| CN109847755A (en) * | 2019-04-01 | 2019-06-07 | 郑州大学 | A kind of novel biomass base catalyst and preparation method thereof and the application in terms of pyrolyzing coal |
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| CN110935453A (en) * | 2019-12-16 | 2020-03-31 | 山东科技大学 | Dolomite catalyst without noble metal and its prepn and use |
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