CN109294631B - Method for preparing bio-oil by catalytic liquefaction of microalgae - Google Patents
Method for preparing bio-oil by catalytic liquefaction of microalgae Download PDFInfo
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Abstract
The invention discloses a method for preparing bio-oil by catalytic liquefaction of microalgae, which comprises the following steps: (1) adding haematococcus, solvent methanol and a transition metal ion-loaded montmorillonite catalyst into a heatable reactor according to a certain proportion for reaction at the temperature of 180 ℃ and the temperature of 240 ℃ for 1-3h, wherein the material-liquid ratio of the haematococcus to the methanol is 0.1-0.5g/mL, and the mass ratio of the haematococcus to the catalyst is 1: 0.01-0.1; (2) naturally cooling to room temperature after the reaction is finished, carrying out suction filtration on the reaction liquid, and collecting a liquid-phase product; (3) and distilling off the solvent methanol and low boiling point substances of the liquid phase product to obtain the bio-oil. The montmorillonite catalyst used in the invention has the advantages of wide source, low price and the like. The yield of the biological oil prepared by the invention is more than 87%, the selectivity is more than 94%, and the calorific value is more than 36 MJ/kg. The method has the advantages of high yield of the biological oil, high product selectivity, high product calorific value and the like.
Description
Technical Field
The invention belongs to the field of catalysis, and particularly relates to a method for preparing bio-oil by carrying out microalgae catalytic liquefaction on a modified montmorillonite catalyst.
Background
With the development of industrialization, the demand of human society for energy is increasing day by day, but the fossil energy reserves are limited, so that the development of an alternative energy is imminent, and biomass energy gradually enters the visual field of people with the advantages of being renewable, large in reserves, harmless to the environment, economically feasible and the like. In a broad sense, biomass is any organic substance formed by photosynthesis of green plants, either directly or indirectly. Biomass is, in a narrow sense, organic matter derived from plants, trees, crops, algae. Currently, although motor vehicle fuels derived from biomass are mainly bioethanol and biodiesel, these biomass fuels have many problems such as limited production areas and low production per unit area, which are caused by using food crops as raw materials, and therefore, in order to secure future supply of motor vehicle fuels, it is necessary to produce liquid fuels in consideration of biomass other than food crops. Microalgae are favored in research because of the characteristics of no competition with grains for land and people, wide distribution, short growth period, high oil content and the like.
At present, the preparation of bio-oil by microalgae is mainly divided into two methods, namely a rapid pyrolysis method and a direct liquefaction method. Compared with the fast pyrolysis method, the direct liquefaction has the following advantages: (1) the raw materials do not need to be dried, so that the energy consumption is greatly reduced; (2) the sub-supercritical solvent system has strong solubility to organic matters. The mass transfer resistance is small, which is beneficial to the full liquefaction of the microalgae. At present, direct liquefaction is receiving a great deal of attention and has gradually become the mainstream research direction in this field.
CN107629812A discloses a method for preparing bio-oil by hydrothermal liquefaction, which comprises the steps of adding sludge and water into a reaction kettle, reacting under an oxygen-free condition, wherein the reaction temperature is 300-320 ℃, the reaction time is 20min, the bio-oil yield is 37.6%, the heat value reaches 35.2MJ/kg, but the reaction temperature is too high, the bio-oil yield is low, the selectivity is poor, the requirement on equipment is high, and the method is not beneficial to industrial application.
CN105772076B discloses a method for preparing bio-oil by using a hydrothermal stable mesoporous molecular sieve as a catalyst, which uses microalgae as a raw material, water as a solvent, and a mesoporous molecular sieve as a catalyst. The liquefaction temperature is 240-320 ℃, the pressure is 5-18 MPa, and the reaction time is 10-45 min. The method has high reaction temperature and reaction pressure, and is not beneficial to industrial application.
CN103484234B discloses a method for preparing bio-oil by catalytic liquefaction of microalgae, which comprises the step of reacting microalgae, acetone and a catalyst, wherein the catalyst mainly comprises inorganic salts such as zinc chloride, sodium trifluoromethanesulfonate, ferric chloride and stannic chloride, and the liquefaction temperature is 270-350 ℃. The method has high reaction temperature, the catalyst is not easy to separate, and a large amount of three wastes are generated.
CN102002381B discloses a method for preparing bio-oil by catalytic liquefaction of microalgae, which comprises the steps of soaking the microalgae in alkali liquor for 20 hours, adding the soaked solution and a modified natural mordenite catalyst into a reaction kettle, and filling hydrogen for pressurized reaction at the reaction temperature of 200-400 ℃. The method uses alkali liquor for pretreatment and reaction, the alkali can remain in the bio-oil to cause the quality of the bio-oil to be reduced, and meanwhile, the reaction process can corrode equipment, thereby being not beneficial to industrial application.
In summary, the methods for preparing bio-oil reported at present have many defects, or the bio-oil yield is low, the selectivity is poor, or the reaction conditions are harsh, or the equipment is severely corroded, etc. Therefore, it is very important to develop a method for preparing bio-oil with low cost, relatively mild reaction conditions and clean process.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for preparing bio-oil by catalytic liquefaction of microalgae.
The technical scheme of the invention is as follows:
a method for preparing bio-oil by catalytic liquefaction of microalgae comprises the following steps:
(1) dissolving a certain amount of transition metal salt in distilled water, adding montmorillonite, stirring at room temperature for 4-8 hours, wherein the mass ratio of the transition metal salt to the montmorillonite is 1: 0.5-8, forming a uniform and stable solid-liquid mixture, performing suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, performing vacuum drying at 100-130 ℃ for 3-10 hours, grinding the filter cake, and calcining at 200-500 ℃ to obtain a catalyst;
(2) adding haematococcus, methanol and the prepared catalyst into a heatable reactor for reaction, wherein the feed-liquid ratio of the haematococcus to the methanol is 0.05-1.0 g/mL; the mass ratio of the haematococcus pluvialis to the catalyst is 1: 0.005 to 0.5; the reaction temperature is 150-270 ℃, and the reaction time is 0.5-5 h; naturally cooling to room temperature after the reaction is finished, carrying out suction filtration on the reaction liquid, and collecting a liquid-phase product; and (4) evaporating the solvent methanol and low boiling point substances of the liquid phase product to obtain the bio-oil product. The reaction temperature is 180-240 ℃, and the reaction time is 1-3 h; the feed-liquid ratio of haematococcus alga to methanol is 0.1-0.5g/mL, and the mass ratio of haematococcus alga to catalyst is 1: 0.01 to 0.1;
in a preferred embodiment of the invention, the metal salt is NiCl2，CoCl2，Mo(NO3)3，FeCl3，MnCl2，CuCl2One kind of (1).
In a preferred embodiment of the invention, the mass ratio of the metal salt to the montmorillonite is 1: 1-5.
In a preferred embodiment of the present invention, the reaction temperature is 220 to 240 ℃.
In a preferred embodiment of the present invention, the reaction time is 1 h.
In a preferred embodiment of the present invention, the feed-to-liquid ratio of Haematococcus to methanol is 0.2 g/mL.
In a preferred embodiment of the present invention, the mass ratio of haematococcus pluvialis to catalyst is 1: 0.05.
in a preferred embodiment of the present invention, low boiling point material means material having a boiling point below 70 ℃.
The invention has the beneficial effects that:
(1) the microalgae used in the invention does not need drying treatment, the energy consumption in the production process is lower, and the production cost can be greatly reduced.
(2) The catalyst of the invention is modified montmorillonite which has wide source, low price and easy recovery and reuse.
(3) The whole process is simple, convenient to operate, low in reaction temperature, mild in reaction condition and low in energy consumption, further reduces the production cost, and has an industrial application prospect.
(4) The biological oil yield is more than 87%, and the selectivity is more than 94%.
Detailed Description
The technical solutions of the invention are further illustrated and described below with reference to specific embodiments.
Catalyst preparation
Example one
10g of NiCl2Dissolving in distilled water, adding 15g of montmorillonite, stirring at room temperature for 5h to form a uniform and stable solid-liquid mixture, carrying out suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, then carrying out vacuum drying at 120 ℃ for 5h, finally grinding the filter cake, and calcining at 400 ℃ to obtain the catalyst.
Example two
10g of CoCl2Dissolving in distilled water, adding 15g of montmorillonite, stirring at room temperature for 5h to form a uniform and stable solid-liquid mixture, carrying out suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, then carrying out vacuum drying at 120 ℃ for 5h, finally grinding the filter cake, and calcining at 400 ℃ to obtain the catalyst.
EXAMPLE III
10g of Mo (NO)3)3Dissolving in distilled water, adding 15g of montmorillonite, stirring at room temperature for 5h to form a uniform and stable solid-liquid mixture, carrying out suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, then carrying out vacuum drying at 120 ℃ for 5h, finally grinding the filter cake, and calcining at 400 ℃ to obtain the catalyst.
Example four
10g of FeCl3Dissolving in distilled water, adding 15g of montmorillonite, stirring at room temperature for 5h to form a uniform and stable solid-liquid mixture, carrying out suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, then carrying out vacuum drying at 120 ℃ for 5h, finally grinding the filter cake, and calcining at 400 ℃ to obtain the catalyst.
EXAMPLE five
10g of MnCl2Dissolving in distilled water, adding 15g of montmorillonite, stirring at room temperature for 5h to form a uniform and stable solid-liquid mixture, carrying out suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, then carrying out vacuum drying at 120 ℃ for 5h, finally grinding the filter cake, and calcining at 400 ℃ to obtain the catalyst.
EXAMPLE six
10g of CuCl2Dissolving in distilled water, adding 15g of montmorillonite, stirring at room temperature for 5h, and shapingForming a uniform and stable solid-liquid mixture, carrying out suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, then carrying out vacuum drying at 120 ℃ for 5h, finally grinding the filter cake, and calcining at 400 ℃ to obtain the catalyst.
Production example of bio-oil
EXAMPLE seven
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Ni-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 240 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 84.1%, the liquefaction rate is 94.7%, the selectivity is 88.8%, and the heat value of the bio-oil is 36.3 +/-0.04 MJ/kg.
Example eight
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Cu-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 240 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 87.4%, the liquefaction rate is 92.9%, the selectivity is 94.4%, and the heat value of the bio-oil is 35.41 +/-0.03 MJ/kg.
Example nine
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Fe-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 240 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 86.5%, the liquefaction rate is 90.6%, the selectivity is 94.4%, and the heat value of the bio-oil is 35.61 +/-0.07 MJ/kg.
Example ten
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Mn-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 240 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 87.2%, the liquefaction rate is 92.3%, the selectivity is 94.5%, and the heat value of the bio-oil is 34.63 +/-0.04 MJ/kg.
EXAMPLE eleven
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Mo-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 240 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 86.3%, the liquefaction rate is 93.3%, the selectivity is 92.4%, and the heat value of the bio-oil is 34.82 +/-0.06 MJ/kg.
Example twelve
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Co-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 240 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 85.4%, the liquefaction rate is 96.3%, the selectivity is 88.7%, and the heat value of the bio-oil is 34.91 +/-0.04 MJ/kg.
EXAMPLE thirteen
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Ni-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 220 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 78.9%, the liquefaction rate is 86.3%, the selectivity is 91.4%, and the heat value of the bio-oil is 34.16 +/-0.03 MJ/kg.
Example fourteen
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Co-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 220 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 79.2%, the liquefaction rate is 88.4%, the selectivity is 89.6%, and the heat value of the bio-oil is 35.25 +/-0.08 MJ/kg.
Example fifteen
Adding 50mL of methanol, 10g of haematococcus pluvialis and 0.5g of Mo-loaded montmorillonite catalyst into a reaction kettle, sealing the reaction kettle, adjusting a controller to enable the temperature of the reaction kettle to rise to 220 ℃, and reacting for 60min at the temperature. And after the reaction kettle is cooled to room temperature, collecting the mixture in the reaction kettle, and performing suction filtration on the reaction product to obtain a solid-phase product and a liquid-phase product. And (3) evaporating the methanol from the liquid-phase product to obtain the bio-oil finally, and drying the solid-phase product to obtain solid-phase residue. The yield of the bio-oil obtained by the experiment is 77.. 9%, the liquefaction rate is 88.4%, the selectivity is 88.1%, and the heat value of the bio-oil is 35.03 +/-0.02 MJ/kg.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Attached:
the calculation formulas of the yield, the liquefaction rate, the selectivity and the calorific value of the bio-oil are as follows:
the calorific value of the bio-oil is 0.3404C +0.0628N-0.0984O
Wherein C, H and O are the mass percentage contents of carbon element, hydrogen element and oxygen element in the biological oil respectively.
Claims (6)
1. A method for preparing bio-oil by catalytic liquefaction of microalgae is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a catalyst: dissolving a certain amount of transition metal salt in distilled water, adding montmorillonite, stirring at room temperature for 4-8 hours, wherein the mass ratio of the transition metal salt to the montmorillonite is 1: 0.5-8, forming a uniform and stable solid-liquid mixture, performing suction filtration on the obtained solid-liquid mixture, washing a filter cake with distilled water, performing vacuum drying at 100-130 ℃ for 3-10 hours, grinding the filter cake, and calcining at 200-500 ℃ to obtain a catalyst; the transition metal salt is CoCl2，Mo(NO3)3，FeCl3，MnCl2，CuCl2At least one of;
(2) preparing the bio-oil: adding haematococcus, methanol and a prepared catalyst into a heatable reactor for reaction, wherein the feed-liquid ratio of the haematococcus to the methanol is 0.05-1.0 g/mL; the mass ratio of the haematococcus pluvialis to the catalyst is 1: 0.005 to 0.5; the reaction temperature is 150-240 ℃, and the reaction time is 0.5-5 h; naturally cooling to room temperature after the reaction is finished, carrying out suction filtration on the reaction liquid, and collecting a liquid-phase product; and (4) evaporating the solvent methanol and low boiling point substances of the liquid phase product to obtain the bio-oil product.
2. The method for preparing bio-oil by catalytic liquefaction of microalgae according to claim 1, wherein: the mass ratio of the transition metal salt to the montmorillonite is 1: 1-5.
3. The method for preparing bio-oil by catalytic liquefaction of microalgae according to claim 1, wherein: the reaction temperature is 180-240 ℃, and the reaction time is 1-3 h.
4. The method for preparing bio-oil by catalytic liquefaction of microalgae according to claim 1, wherein: the feed-liquid ratio of haematococcus pluvialis to methanol is 0.1-0.5 g/mL.
5. The method for preparing bio-oil by catalytic liquefaction of microalgae according to claim 1, wherein: the mass ratio of the haematococcus pluvialis to the catalyst is 1: 0.01 to 0.1.
6. The method for preparing bio-oil by catalytic liquefaction of microalgae according to claim 1, wherein: low boiling point material means material having a boiling point below 70 ℃.
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