CN103316647A - Method for preparing supported solid-base catalyst and bio-oil - Google Patents
Method for preparing supported solid-base catalyst and bio-oil Download PDFInfo
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- CN103316647A CN103316647A CN2013102778624A CN201310277862A CN103316647A CN 103316647 A CN103316647 A CN 103316647A CN 2013102778624 A CN2013102778624 A CN 2013102778624A CN 201310277862 A CN201310277862 A CN 201310277862A CN 103316647 A CN103316647 A CN 103316647A
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Abstract
The invention discloses a method for preparing supported solid-base catalyst and bio-oil. The bio-oil is prepared from biomass through catalytic vacuum cracking reaction in a tube-type furnace reactor in the presence of the supported solid-base M/gamma-Al2O3 catalyst (wherein M is Ca, Mg, Na, K) under the condition that the reaction temperature is 450 to 600 DEG C and the pressure is (-0.1)MPa. The mass ratio of the catalyst to the biomass is (1:10) to (1:25). The preparation method is simple; after being applied to the biomass cracking, the prepared supported catalyst can effectively improve the yield of the bio-oil.
Description
Technical field
The present invention relates to a kind of method of bio oil, particularly a kind of load type solid body base catalyst catalysis vacuum cracking living beings are produced the method for bio oil.
Background technology
Day by day in short supply along with fossil energy, people are also more and more deep to the research of various regenerative resources, and wherein biomass energy is with its hypotoxicity, low pollute and reserves are abundant begins to be subject to people and pay close attention to.China utilizes regenerative resource to improve present situation as populous nation, large agricultural country, energy consumption big country, has more realistic meaning.
Biomass thermal chemical conversion technology is a kind of of Biomass Energy Utilization technology, wherein vacuum cracking is a kind of technology take the liquid phase bio oil as the main target product, this technology makes living beings be converted under certain vacuum degree and temperature can not coagulate combustion gas, three kinds of energy forms of bio oil and coke.Living beings at high temperature at first change into fugitive constituent, and this fugitive constituent is converted into bio oil and can not coagulates combustion gas by behind the condensing unit.Patent CN101343547A discloses a kind of method of vacuum cracking classification preparing bio-oil, but the limitations restrict of condensing unit design the productive rate of bio oil, and whole system is in negative pressure state, this online sampling for sample is difficult to realize.The condensation of the disclosed cracked oil condensation method of CN1030252A takes time one-level condensate liquid to the previous stage condensation, may cause polymerization even the coking of part low boiling heat-sensitive substance.At present, the general yield of biomass through pyrolysis method is lower, can improve the bio oil yield by catalysis.Patent CN101508619A discloses the method for a kind of living beings and polymer preparing hydrocarbon with catalysis copyrolysis, but catalyst system therefor to be damaged tire, poly-second uncommon and daily waste plastic etc., the catalyst raw material is various, and needs again to process; This is difficult to Effective Raise bio oil productive rate also so that the bio oil composition is more complicated.
Summary of the invention
Technical problem:The invention provides and a kind ofly prepare simply, the product catalytic performance is good, and the method for preparing load type solid body base catalyst that can Effective Raise bio oil yield provides a kind of method for preparing bio oil simultaneously.
Technical scheme:The method for preparing load type solid body base catalyst of the present invention may further comprise the steps:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h;
2) choose in magnesium nitrate, calcium nitrate, sodium carbonate, the potash any, be dissolved in the deionized water, be made into the metal salt solution that concentration is 0.2 ~ 0.4mol/L, with the γ-Al of drying in the step 1)
2O
3Carrier impregnation in metal salt solution, slaine and γ-Al
2O
3Mass ratio 1:4~1:10, dip time 48h;
3) with step 2) in process the suspension obtain and behind suction filtration, obtain γ-Al
2O
3Carrier is dried under 90 ~ 150 ℃ of conditions, in 400 ~ 600 ℃ of calcining 3 ~ 10h, obtains powdery solid, namely obtains the load type solid body base catalyst for the biomass vacuum cracking.
The method for preparing bio oil of the present invention is come preparing bio-oil by catalysis vacuum cracking living beings, specifically comprises the steps:
1) the white poplar wood chip is filtered into 40~100 purpose particles, puts into vacuum drying chamber and dry by the fire 10h;
2) will be according to the method described above processing obtains in prepared load type solid body base catalyst and the step 1) white poplar wood chip in mass ratio 1:10~1:25 evenly mix;
3) with step 2) in process the mixture obtain and put into tube furnace, cracking 0.5~2h under 450 ~ 600 ℃, vacuum condition, the gas of generation is collected by-20~0 ℃ of cold hydrazine condensation, namely obtains bio oil.
Beneficial effect:The relative prior art of the present invention has the following advantages:
At first, load type solid body base catalyst preparation is simple, compares self-catalyzed reaction, and preparation condition that can the Effective Regulation catalyst is with the impact of research on reaction, and obtains optimal conditions.
Secondly, the main component of load type solid body base catalyst is the oxide of calcium metal, magnesium, sodium, potassium, has avoided the use of rare precious metals and toxic metals, not only environmental protection but also significantly reduced production cost; And this catalyst has higher catalytic efficiency, and the bio oil yield can reach 59.64%.
At last, adopt the vacuum environment cracking, can reduce the cracking temperature of living beings, quick collection cracking gas and condensation obtain bio oil; The adding of catalyst has improved the yield of bio oil greatly.
The specific embodiment
The present invention will be further described below by embodiment.
Embodiment 1:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 26.0g; γ-Al
2O
3That crystal formation is the aluminium oxide of γ type.
2) prepare to take by weighing Mg (NO
3)
26H
2O 2.6g is dissolved in the 50mL deionized water, with the 26.0g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 400 ℃ the calcining 3h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
Evenly add in tube furnace with the 2g catalyst mix 50g poplar bits, utilize oil pump with the pressure state that is evacuated, with diamond heating to 450 ℃, the rate of heat addition is 10 ℃/min again, reaction time 0.5h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtain bio oil 19.56g, carbon residue 12.33g, cracking gas 18.11g.The bio oil yield is 39.12%.
Embodiment 2:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 20.8g;
2) prepare to take by weighing Mg (NO
3)
26H
2O 5.2g is dissolved in the 50mL deionized water, with the 10.0g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 600 ℃ the calcining 10h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
50g poplar bits and 5g catalyst are evenly mixed in the adding tube furnace, utilize oil pump with the pressure state that is evacuated, with diamond heating to 600 ℃, the rate of heat addition is 10 ℃/min again, reaction time 2h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtaining bio oil is 23.16g, and carbon residue is 10.27g, and cracking gas is 16.57g.The bio oil yield is 46.32%.
Embodiment 3:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 24.0g;
2) prepare to take by weighing Ca (NO
3)
24H
2O 2.4g is dissolved in the 50mL deionized water, with the 24.0g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 400 ℃ the calcining 3h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
50g poplar bits and 3g catalyst are evenly mixed in the adding tube furnace, utilize oil pump with the pressure state that is evacuated, with diamond heating to 450 ℃, the rate of heat addition is to react under the 10 ℃/min condition again, reaction time 1h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtain bio oil 22.87g, carbon residue 9.14g, cracking gas 17.99g.The bio oil yield is 45.74%.
Embodiment 4:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 19.2g;
2) prepare to take by weighing Ca (NO
3)
24H
2O 4.8g is dissolved in the 50mL deionized water, with the 19.2g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 600 ℃ the calcining 10h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
50g poplar bits and 5g catalyst are evenly mixed in the adding tube furnace, utilize oil pump with the pressure state that is evacuated, with diamond heating to 600 ℃, the rate of heat addition is to react under the 10 ℃/min condition again, reaction time 2h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtain bio oil 22.36g, carbon residue 8.82g, cracking gas 18.82g.The bio oil yield is 44.72%.
Embodiment 5:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 28.8g;
2) prepare to take by weighing Ca (NO
3)
24H
2O 4.8g is dissolved in the 50mL deionized water, with the 28.8g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 500 ℃ the calcining 5h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
50g poplar bits and 4g catalyst are evenly mixed in the adding tube furnace, utilize oil pump with the pressure state that is evacuated, with diamond heating to 550 ℃, the rate of heat addition is to react under the 10 ℃/min condition again, reaction time 1.5h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtaining bio oil is 25.36g, and carbon residue is 9.43g, and cracking gas is 15.21g.The bio oil yield is 50.72%.
Embodiment 6:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 28.8g;
2) prepare to take by weighing Ca (NO
3)
24H
2O 3.6g is dissolved in the 50mL deionized water, with the 28.8g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 550 ℃ the calcining 6h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
50g poplar bits and 4g catalyst are evenly mixed in the adding tube furnace, utilize oil pump with the pressure state that is evacuated, with diamond heating to 500 ℃, the rate of heat addition is to react under the 10 ℃/min condition again, reaction time 1h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtaining bio oil is 29.82g, and carbon residue is 8.57g, and cracking gas is 11.61g.The bio oil yield is 59.64%.
Embodiment 7:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 25.2g;
2) prepare to take by weighing Ca (NO
3)
24H
2O 3.6g is dissolved in the 50mL deionized water, with the 25.2g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 600 ℃ the calcining 7h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
50g poplar bits and 5g catalyst are evenly mixed in the adding tube furnace, utilize oil pump with the pressure state that is evacuated, with diamond heating to 500 ℃, the rate of heat addition is to react under the 10 ℃/min condition again, reaction time 1.5h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtaining bio oil is 26.10g, and carbon residue is 10.03g, and cracking gas is 13.87g.The bio oil yield is 52.20%.
Embodiment 8:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 11.0g;
2) prepare to take by weighing Na
2CO
31.1g, be dissolved in the 50mL deionized water, with the 11.0g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 400 ℃ the calcining 10h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
Evenly add in tube furnace with the 2g catalyst mix 50g poplar bits, utilize oil pump with the pressure state that is evacuated, with diamond heating to 450 ℃, the rate of heat addition is 10 ℃/min again, reaction time 0.5h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtain bio oil 20.56g, carbon residue 13.33g, cracking gas 16.11g.The bio oil yield is 41.12%.
Embodiment 9:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 8.8g;
2) prepare to take by weighing Na
2CO
32.2g, be dissolved in the 50mL deionized water, with the 8.8g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 600 ℃ the calcining 3h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
Evenly add in tube furnace with the 2g catalyst mix 50g poplar bits, utilize oil pump with the pressure state that is evacuated, with diamond heating to 600 ℃, the rate of heat addition is 10 ℃/min again, reaction time 2h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtain bio oil 21.02g, carbon residue 12.13g, cracking gas 16.85g.The bio oil yield is 39.12%.
Embodiment 10:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 14.0g;
2) prepare to take by weighing K
2CO
31.4g, be dissolved in the 50mL deionized water, with the 14.0g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 400 ℃ the calcining 10h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
Evenly add in tube furnace with the 2g catalyst mix 50g poplar bits, utilize oil pump with the pressure state that is evacuated, with diamond heating to 450 ℃, the rate of heat addition is 10 ℃/min again, reaction time 2h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtain bio oil 19.56g, carbon residue 12.33g, cracking gas 18.11g.The bio oil yield is 39.12%.
Embodiment 11:
(1) preparation process of catalyst:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h, prepares to take by weighing this solid particle of 11.2g;
2) prepare to take by weighing K
2CO
32.8g, be dissolved in the 50mL deionized water, with the 11.2g γ-Al of described step 1)
2O
3Be impregnated in the metal salt solution dip time 48h;
3) with described step 2) the middle γ-Al that obtains that processes
2O
3Suction filtration dries by the fire 24h in the baking oven under 90 ℃ of conditions, to remove moisture wherein, at last in Muffle furnace in 600 ℃ the calcining 3h, obtain blocks of solid; The gained blocks of solid is ground to 80 ~ 120 orders, namely gets the catalyst for catalysis vacuum cracking living beings.
(2) preparation of bio oil
Evenly add in tube furnace with the 5g catalyst mix 50g poplar bits, utilize oil pump with the pressure state that is evacuated, with diamond heating to 600 ℃, the rate of heat addition is 10 ℃/min again, reaction time 0.5h, cracking gas carries out collecting biological oil by-20 ℃ of glass cold hydrazines.Obtain bio oil 20.73g, carbon residue 13.49g, cracking gas 15.78g.The bio oil yield is 41.46%.
In addition to the implementation, all employings are equal to the technical scheme of replacement or equivalent transformation formation, the protection domain that all requires in the present invention.
Claims (2)
1. method for preparing load type solid body base catalyst, it is characterized in that: the method comprises the steps:
1) with γ-Al
2O
3Carrier grinds to form 80 ~ 120 purpose particles, puts into baking oven and dries by the fire 12h;
2) choose in magnesium nitrate, calcium nitrate, sodium carbonate, the potash any, be dissolved in the deionized water, be made into the metal salt solution that concentration is 0.2 ~ 0.4mol/L, with the γ-Al of drying in the described step 1)
2O
3Carrier impregnation in metal salt solution, slaine and γ-Al
2O
3Mass ratio 1:4~1:10, dip time 48h;
3) with described step 2) in process the suspension obtain and behind suction filtration, obtain γ-Al
2O
3Carrier is dried under 90 ~ 150 ℃ of conditions, in 400 ~ 600 ℃ of calcining 3 ~ 10h, obtains powdery solid, namely obtains the load type solid body base catalyst for the biomass vacuum cracking.
2. a method for preparing bio oil is characterized in that, the method is come preparing bio-oil by catalysis vacuum cracking living beings, specifically comprises the steps:
1) the white poplar wood chip is filtered into 40~100 purpose particles, puts into vacuum drying chamber and dry by the fire 10h;
The white poplar wood chip that 2) will obtain according to processing in the load type solid body base catalyst of the described method of claim 1 preparation and the described step 1) in mass ratio 1:10~1:25 evenly mixes;
3) with described step 2) in process the mixture obtain and put into tube furnace, cracking 0.5~2h under 450 ~ 600 ℃, vacuum condition, the gas of generation is collected by-20~0 ℃ of cold hydrazine condensation, namely obtains bio oil.
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Cited By (2)
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CN109621936A (en) * | 2018-12-13 | 2019-04-16 | 南京农业大学 | A kind of CaO- charcoal dehydrogenation catalyst and its method for being catalyzed oil compounds liquid fuel was prepared |
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Cited By (2)
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CN109621936A (en) * | 2018-12-13 | 2019-04-16 | 南京农业大学 | A kind of CaO- charcoal dehydrogenation catalyst and its method for being catalyzed oil compounds liquid fuel was prepared |
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Application publication date: 20130925 |