CN103773589A - Method for preparing biologic oil from blue algae in catalytic cracking mode in vacuum - Google Patents
Method for preparing biologic oil from blue algae in catalytic cracking mode in vacuum Download PDFInfo
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- CN103773589A CN103773589A CN201410017836.2A CN201410017836A CN103773589A CN 103773589 A CN103773589 A CN 103773589A CN 201410017836 A CN201410017836 A CN 201410017836A CN 103773589 A CN103773589 A CN 103773589A
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Abstract
The invention discloses a method for preparing biologic oil from blue algae in a catalytic cracking mode in vacuum. The biologic oil is prepared by taking blue alga powder as a raw material and a composite metal oxide which takes hydrotalcite as a precursor as a catalyst in the catalytic cracking mode in vacuum. The method takes the composite metal oxide as the catalyst, so that the preparation is simple to carry out; by applying the prepared catalyst to blue alga cracking, the yield of the biologic oil can be effectively improved; moreover, as the metal oxide can absorb the moisture in the blue algae, the quality of the biologic oil is improved. The method disclosed by the invention is simple, the blue algae which is the chief culprit of eutrophication to a water body is taken as the raw material, the waste is turned into wealth, and the environment pollution is alleviated.
Description
Technical field
The present invention relates to the treatment process of a kind of blue-green algae, particularly a kind of method take complex metal oxides as catalyzer vacuum catalytic cracking blue-green algae preparing bio-oil.
Background technology
Blue-green algae be domestic and the planktonic algae that produces of a lot of inland lake eutrophication in the world in most important one, it is present in water body, bring infinite harm to people, for example, destroyed the healthy of the ecosystem, polluted source harm humans and discharge odor pollution air etc.Salvaging is the common measure that pollution that China causes for lake wawter bloom is taked, and is used by normalization in China Dian Chi, Taihu Lake, Chaohu etc.According to incompletely statistics, within 2011,970,000 tons of blue algae liquid are salvaged from Taihu Lake accumulative total by Jiangsu Province, increase nearly 300,000 tons than salvaging amount in 2010.And these salvage the blue algae liquid of disembarkation, how in time, harmless treatment fast and utilization, be the key that bloom blue algae is administered.If to the blue-green algae of salvaging can not be in time, harmless treatment effectively, the environmental pollution that can produce secondary because of releases such as rotten smelly, the nitrogen of blue-green algae, phosphorus nutrients.
At present, domestic to salvage blue-green algae mainly adopt the method for anaerobic digestion to process, as the patent No. Chinese patent that is 200810022548.0 has been reported a kind of method of anaerobic fermentation of bloom blue algae, improve processing efficiency by shortening digestion time, but can't resolve the key issue of reaction needed long period.Meanwhile, there is a large amount of moisture in the blue algae liquid of salvaging disembarkation, can cause the problems such as anaerobic digester scale is bigger than normal, floor space is large.
In addition, also the blue algae liquid of useful salvaging disembarkation is prepared fertilizer, is built the methods such as microbiological fuel cell, but all deposit particular problem on the implementation, as prepare fertilizer and the blue algae liquid of salvaging disembarkation need to be carried out to second dehydration, when high-moisture percentage, its processing rate is low.
In addition, also have patent report supercritical water treatment blue algae liquid, the Chinese patent that the patent No. is 201010520895.3, has reported and has taked the reactive mode of supercritical water oxidation that blue-green algae is converted into CO
2and H
2o.And this kind of method be owing to adding oxygenant in reaction process, its main purpose is to realize the harmless treatment of blue algae liquid, and cost is higher, and does not consider the transition problem of the energy; Because need dehydration before blue-green algae reaction, technique is more complicated again.
Investigator prepares bio oil take blue-green algae as raw material both at home and abroad, mainly adopts the thermochemistry transformation technology of rapidly pyrolysing and liquefying and direct liquefaction.At present, blue-green algae is prepared bio oil very large difficulty, exists the series of problems such as the imperfection of technology, oily productive rate are not high, production cost is high, oil quality is low.
Summary of the invention
The object of this invention is to provide a kind of method of blue-green algae vacuum catalytic cracking preparing bio-oil, prepare the problems such as bio oil oil productive rate is not high, production cost is high, oil quality is low to solve existing blue-green algae.
For addressing the above problem, the present invention by the following technical solutions:
A method for blue-green algae vacuum catalytic cracking preparing bio-oil, take blue-green algae powder as raw material, the complex metal oxides that hydrotalcite is presoma is catalyzer, under vacuum, catalytic pyrolysis is produced bio oil, comprises the steps:
Step 1, after being calcined to 1～5h at 300～600 ℃, hydrotalcite obtains complex metal oxides;
Step 2, complex metal oxides prepared by step 1 and blue-green algae powder in mass ratio 0.5～2:10 mix;
Step 3, the mixture that step 2 is obtained are put into tube furnace, and vacuum tightness is 50～100kPa, at 100～200 ℃, stop 20～60min, temperature is increased to 400～600 ℃ afterwards, cracking 0.5～2h, passes through-20～0 ℃ of cold hydrazine condensations by the splitting gas of generation, collects and obtains bio oil.
Described in step 1, hydrotalcite is one or more in Mg-Al hydrotalcite, Ca-Mg-Al hydrotalcite, Zn-Mg-Al hydrotalcite.
Beneficial effect of the present invention:
1, the present invention, take arch-criminal-blue-green algae of causing body eutrophication as waste bio oil, is turned waste into wealth, and reduces environmental pollution.Simple, the oily productive rate of the inventive method technique is high.
2, the catalyzer that the present invention uses is complex metal oxides, and preparation is simple; The catalyzer of preparation is applied to blue-green algae cracking, can effectively improves the productive rate of bio oil; And metal oxide can absorb the moisture in blue-green algae, the quality of lifting bio oil.
3, the main component of complex metal oxides is the oxide compound of MAGNESIUM METAL, aluminium, calcium, zinc, has avoided the use of rare precious metals and toxic metal, not only environmental protection but also significantly reduced production cost; And this catalyzer has higher catalytic efficiency, bio oil yield can reach 65.7%.
4, adopt vacuum environment cracking, can reduce the cracking temperature of biomass, quick collection splitting gas condensation obtain bio oil.
Embodiment
Below in conjunction with embodiment, the present invention is done further and explained.The following example is only for the present invention is described, but is not used for limiting practical range of the present invention.
The preparation method of the Mg-Al hydrotalcite that following examples are used is as follows:
Step 1, get magnesium nitrate and aluminum nitrate in molar ratio 3:1 add in 1L beaker, add deionized water and stirring even;
Step 2, get sodium hydroxide and sodium carbonate in molar ratio 1:1 add in 1L beaker, add deionized water and stirring even;
Step 3, the mixing solutions that processing in described step 1,2 is obtained are transferred to respectively constant pressure funnel, are added drop-wise in the 2L beaker that adds a certain amount of deionized water simultaneously, constantly regulate flow velocity in dropping process, guarantee that the pH value of mixed solution is between 9～11;
Step 4, dropwise rear continuation and stir for some time, then thermostatic crystallization at 40～100 ℃, in 400～600 ℃ of calcining 2～5h, grind into powder after solid drying, particle diameter is less than 0.2mm.
The preparation method of Ca-Mg-Al hydrotalcite and Zn-Mg-Al hydrotalcite is the same, just raw material and material molar ratio difference, and preparation Ca-Mg-Al hydrotalcite raw material and material molar ratio used is: Ca:Mg:Al=3:3:2, NaOH:Na
2cO
3=4:1, preparation Zn-Mg-Al hydrotalcite raw material and material molar ratio used is: Zn:Mg:Al=3:2:2, NaOH:Na
2cO
3=3:1.
Embodiment blue-green algae powder used is that the Exposure to Sunlight of blue-green algae process, the vacuum drying oven that are salvaged by Taihu Lake are dry, Universalpulverizer is pulverized, filtered out through 40～100 object standard sieves the powder that particle diameter is 150 microns of left and right again, gained after 60～100 ℃ of dry 2～6h.
Embodiment 1
Mg-Al hydrotalcite is calcined to 1h at 300 ℃, get after 0.5g product mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 100kPa, stop 60min at 100 ℃, with the heating rate of 10 ℃/min, temperature is risen to 400 ℃ afterwards, cracking 0.5h, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.23g, carbon residue 2.42g, splitting gas 1.35g.Bio oil yield is 62.3%.
Embodiment 2
Ca-Mg-Al hydrotalcite is calcined to 3h at 450 ℃, get after 0.5g product mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 50kPa, stop 20min at 100 ℃, with the heating rate of 10 ℃/min, temperature is risen to 400 ℃ afterwards, cracking 1.0h, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.37g, carbon residue 2.34g, splitting gas 1.29g.Bio oil yield is 63.7%.
Embodiment 3
Mg-Al hydrotalcite is calcined to 5h at 600 ℃, get after 0.5g product mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 100kPa, stop 20min at 100 ℃, with the heating rate of 10 ℃/min, temperature is risen to 400 ℃ afterwards, cracking 1.5h, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.42g, carbon residue 2.35g, splitting gas 1.23g.Bio oil yield is 64.2%.
Embodiment 4
Zn-Mg-Al hydrotalcite is calcined to 3h at 450 ℃, get after 1g product mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 100kPa, stop 40min at 100 ℃, with the heating rate of 10 ℃/min, temperature is risen to 400 ℃ afterwards, cracking 1h, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.47g, carbon residue 2.30g, splitting gas 1.23g.Bio oil yield is 64.7%.
Embodiment 5
After being calcined to 1h at 500 ℃, Mg-Al hydrotalcite gets product 0.2g, after being calcined to 3h at 300 ℃, Ca-Mg-Al hydrotalcite gets product 0.3g, after mixing with 10g blue-green algae powder again, add in tube furnace, vacuum tightness is 100kPa, stop 40min at 100 ℃, temperature is risen to 400 ℃, cracking 1.0h with the heating rate of 10 ℃/min afterwards, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.26g, carbon residue 2.41g, splitting gas 1.33g.Bio oil yield is 62.6%.
Embodiment 6
After being calcined to 1h at 300 ℃, Mg-Al hydrotalcite gets product 0.5g, after being calcined to 3h at 450 ℃, Zn-Mg-Al hydrotalcite gets product 0.5g, after mixing with 10g blue-green algae powder again, add in tube furnace, vacuum tightness is 50kPa, stop 40min at 100 ℃, temperature is risen to 400 ℃, cracking 1.5h with the heating rate of 10 ℃/min afterwards, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.40g, carbon residue 2.28g, splitting gas 1.32g.Bio oil yield is 64.0%.
Embodiment 7
After being calcined to 5h at 450 ℃, Ca-Mg-Al hydrotalcite gets product 1.0g, after being calcined to 1h at 600 ℃, Zn-Mg-Al hydrotalcite gets product 0.5g, after mixing with 10g blue-green algae powder again, add in tube furnace, vacuum tightness is 50kPa, stop 40min at 100 ℃, temperature is risen to 500 ℃, cracking 1.5h with the heating rate of 10 ℃/min afterwards, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.50g, carbon residue 2.28g, splitting gas 1.22g.Bio oil yield is 65.0%.
Embodiment 8
After being calcined to 5h at 450 ℃, Mg-Al hydrotalcite gets product 1.0g, after being calcined to 1h at 450 ℃, Zn-Mg-Al hydrotalcite gets product 1.0g, after mixing with 10g blue-green algae powder again, add in tube furnace, vacuum tightness is 50kPa, stop 60min at 100 ℃, temperature is risen to 500 ℃, cracking 1.5h with the heating rate of 10 ℃/min afterwards, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.55g, carbon residue 2.28g, splitting gas 1.17g.Bio oil yield is 65.5%.
Embodiment 9
After being calcined to 3h at 450 ℃, Ca-Mg-Al hydrotalcite gets product 1.0g, after being calcined to 4h at 500 ℃, Zn-Mg-Al hydrotalcite gets product 0.5g, after mixing with 10g blue-green algae powder again, add in tube furnace, vacuum tightness is 100kPa, stop 40min at 100 ℃, temperature is risen to 450 ℃, cracking 1.5h with the heating rate of 10 ℃/min afterwards, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.57g, carbon residue 2.21g, splitting gas 1.22g.Bio oil yield is 65.7%.
Embodiment 10
Ca-Mg-Al hydrotalcite is calcined to 2h at 600 ℃, get after product 1.5g mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 50kPa, stop 40min at 100 ℃, with the heating rate of 10 ℃/min, temperature is risen to 400 ℃ afterwards, cracking 1.0h, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.41g, carbon residue 2.49g, splitting gas 1.10g.Bio oil yield is 64.1%.
Embodiment 11
Zn-Mg-Al hydrotalcite is calcined to 2h at 300 ℃, get after product 1.5g mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 100kPa, stop 40min at 100 ℃, with the heating rate of 10 ℃/min, temperature is risen to 500 ℃ afterwards, cracking 1h, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.37g, carbon residue 2.25g, splitting gas 1.38g.Bio oil yield is 63.7%.
Embodiment 12
After being calcined to 4h at 500 ℃, Mg-Al hydrotalcite gets product 0.7g, after being calcined to 3h at 400 ℃, Ca-Mg-Al hydrotalcite gets product 0.8g, after being calcined to 2h at 300 ℃, Zn-Mg-Al hydrotalcite gets product 0.5g, after mixing with 10g blue-green algae powder, add in tube furnace, vacuum tightness is 100kPa again, stops 40min at 100 ℃, with the heating rate of 10 ℃/min, temperature is risen to 400 ℃ afterwards, cracking 1.0h, splitting gas passes through-20 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.36g, carbon residue 2.35g, splitting gas 1.29g.Bio oil yield is 63.6%.
Embodiment 13
Mg-Al hydrotalcite is calcined to 1h at 300 ℃, get after 0.5g product mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 100kPa, stop 60min at 150 ℃, with the heating rate of 10 ℃/min, temperature is risen to 600 ℃ afterwards, cracking 2.0h, splitting gas, by the condensation of 0 ℃ of glass cold hydrazine, carries out collecting biological oil.Obtain bio oil 6.18g, carbon residue 2.45g, splitting gas 1.37g.Bio oil yield is 61.8%.
Embodiment 14
Ca-Mg-Al hydrotalcite is calcined to 3h at 450 ℃, get after 0.5g product mixes with 10g blue-green algae powder and add in tube furnace, vacuum tightness is 50kPa, stop 20min at 200 ℃, with the heating rate of 10 ℃/min, temperature is risen to 600 ℃ afterwards, cracking 2.0h, splitting gas passes through-10 ℃ of glass cold hydrazine condensations, carries out collecting biological oil.Obtain bio oil 6.23g, carbon residue 2.42g, splitting gas 1.35g.Bio oil yield is 62.3%.
In addition to the implementation, all employings are equal to the technical scheme of replacement or equivalent transformation formation, the protection domain all requiring in the present invention.
Claims (2)
1. a method for blue-green algae vacuum catalytic cracking preparing bio-oil, is characterized in that, take blue-green algae powder as raw material, the complex metal oxides that hydrotalcite is presoma is catalyzer, and under vacuum, catalytic pyrolysis is produced bio oil, comprises the steps:
Step 1, after being calcined to 1～5h at 300～600 ℃, hydrotalcite obtains complex metal oxides;
Step 2, complex metal oxides prepared by step 1 and blue-green algae powder in mass ratio 0.5～2:10 mix;
Step 3, the mixture that step 2 is obtained are put into tube furnace, and vacuum tightness is 50～100kPa, at 100～200 ℃, stop 20～60min, temperature is increased to 400～600 ℃ afterwards, cracking 0.5～2h, passes through-20～0 ℃ of cold hydrazine condensations by the splitting gas of generation, collects and obtains bio oil.
2. the method for blue-green algae vacuum catalytic cracking preparing bio-oil according to claim 1, is characterized in that, hydrotalcite is one or more in Mg-Al hydrotalcite, Ca-Mg-Al hydrotalcite, Zn-Mg-Al hydrotalcite described in step 1.
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| CN108504377A (en) * | 2018-03-30 | 2018-09-07 | 东南大学 | A method of cyanobacteria catalytic pyrolysis is produced into nitrogen-containing organic compound |
| CN108855101A (en) * | 2016-07-18 | 2018-11-23 | 山东省科学院能源研究所 | Utilize the method for the online improving quality of bio oil of iron-based composite catalyst |
| CN110129086A (en) * | 2019-03-13 | 2019-08-16 | 盐城工业职业技术学院 | A kind of method of catalytic pyrolysis plant asphalt preparation biology boat coal |
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| CN108855101A (en) * | 2016-07-18 | 2018-11-23 | 山东省科学院能源研究所 | Utilize the method for the online improving quality of bio oil of iron-based composite catalyst |
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| CN106753479A (en) * | 2016-12-26 | 2017-05-31 | 山东理工大学 | Biogas fermentation couples the method that Poly-generation processes lignocellulosic with fast pyrogenation |
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| CN108504377B (en) * | 2018-03-30 | 2020-10-16 | 东南大学 | Method for preparing organic nitrogen-containing compound by catalytic thermal cracking of blue algae |
| CN110129086A (en) * | 2019-03-13 | 2019-08-16 | 盐城工业职业技术学院 | A kind of method of catalytic pyrolysis plant asphalt preparation biology boat coal |
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