CN107029727B - Catalyst for catalytic liquefaction of biomass oil and preparation method and application thereof - Google Patents
Catalyst for catalytic liquefaction of biomass oil and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a catalyst for catalyzing and liquefying biomass oil, and a preparation method and application thereof. The preparation method of the catalyst comprises the following steps: (1) mixing a nickel salt solution with titanium dioxide powder, and oscillating to obtain a solid-liquid mixture I; (2) adding a neodymium salt solution into the solid-liquid mixture I in the step 1), and oscillating to obtain a solid-liquid mixture II; (3) and (3) standing the solid-liquid mixture II obtained in the step (2), taking the precipitate, and drying and roasting to obtain the catalyst. The catalyst prepared by the method of the invention can carry out hydrothermal liquefaction reaction on the raw material microalgae powder, and the product oil quality is obviously improved, and the catalytic effect is better. The catalyst for catalyzing and liquefying the biomass oil provided by the invention has the advantages of relieving reaction conditions and improving the yield of product oil in the reaction of preparing the biomass oil by the hydrothermal liquefaction of microalgae, and the heat value of the biomass oil is averagely 31.67MJ/kg and is relatively stable.
Description
Technical Field
The invention relates to the field of biomass engineering and energy, in particular to a catalyst for catalytic liquefaction of microalgae mass oil, a preparation method and application thereof.
Background
With the increasing energy consumption and the worsening of the energy safety situation worldwide, the biomass energy is gradually paid extensive attention, and especially in recent decades, the demand for the biomass energy is rapidly increasing. Among the numerous biomass materials, microalgae are considered promising biomass materials due to their high photosynthetic efficiency, growth rate and yield per unit area. In addition, in fresh water and saline water, microalgae can be cultured on a large scale, and cultivated land and an environment-sensitive zone are not occupied. Therefore, microalgae biomass energy is considered to be a third generation biomass energy.
The theory of petrogeology holds that under natural conditions, there are two types of catalysts, inorganic salts and organic yeast, in the long natural process of organic matter conversion to oil and gas. In the industrial application of the catalyst, the transition metal is loaded on the carrier, and the high dispersity is beneficial to improving the catalytic activity of the catalyst.
Disclosure of Invention
The invention aims to provide a catalyst for catalytic liquefaction of biomass oil and a preparation method and application thereof.
The preparation method of the catalyst provided by the invention comprises the following steps:
1) mixing a nickel salt solution with titanium dioxide powder, and oscillating to obtain a solid-liquid mixture I;
2) adding a neodymium salt solution into the solid-liquid mixture I in the step 1), and oscillating to obtain a solid-liquid mixture II;
3) standing the solid-liquid mixture II obtained in the step 2), taking the precipitate, and drying and roasting to obtain the catalyst.
In the preparation method, the method can further comprise a step of acidifying the titanium dioxide powder before the step 1), specifically a step of adding acid into the titanium dioxide powder and vibrating to obtain a mixed system; the acid may be nitric acid; the acid may be added in the form of an aqueous acid solution, and 30 to 60mL (e.g., 45mL) of the aqueous acid solution is added per 36g of the titanium dioxide powder; the mass percentage of the acid water solution can be 3-10% (such as 5%); the acidification time can be 12-36 hours (such as 24 hours).
In the above preparation method, in step 1), the titanium dioxide powder may be an analytically pure titanium dioxide powder.
In the above preparation method, in step 1), the mass-to-volume ratio of the titania powder to the nickel salt solution may be 1 g: (1-1.5) mL (e.g., 1 g: 1.25 mL); the nickel salt in the nickel salt solution can be nickel chloride; the molar concentration of the nickel salt solution can be 0.24-0.48 g/mL, and specifically can be 0.36 g/mL.
In the preparation method, in the step 1), the oscillation time may be 12 to 36 hours, specifically 24 hours.
In the above preparation method, in step 2), the mass-to-volume ratio of the titanium dioxide powder to the neodymium salt solution may be 1 g: (0.75-3.75) mL, specifically 1 g: 1.25 mL; the neodymium salt in the neodymium salt solution can be neodymium nitrate; the molar concentration of the neodymium salt solution can be 1.00-2.00 mol/L, and specifically can be 1.00-1.50 mol/L, 1.50-2.00 mol/L, 1.00mol/L, 1.50mol/L or 2.00 mol/L.
In the preparation method, in the step 2), the oscillation time may be 12 to 96 hours, specifically 12 to 72 hours, 12 to 24 hours, 24 to 72 hours, 12 hours, 24 hours or 72 hours.
In the preparation method, in the step 3), the drying temperature can be 105-115 ℃, and specifically can be 115 ℃; the time can be 4-12 hours, specifically 8 hours; the roasting temperature can be 200-1000 ℃, specifically 600-800 ℃, 600-675 ℃, 675-800 ℃, 600 ℃, 675 ℃ or 800 ℃, and the time can be 2-9 hours, specifically 3-5 hours, 3-4 hours, 4-5 hours, 3 hours, 4 hours or 5 hours.
The catalyst prepared by the preparation method of any one of the above methods is also in the protection scope of the invention.
The application of the catalyst in at least one of the following 1) to 4) is also within the protection scope of the invention:
1) preparing biomass oil;
2) the yield of the biomass oil is improved;
3) the carbon content of the biomass oil is reduced;
4) the sulfur content of the biomass oil is reduced.
The invention further provides a method for preparing biomass oil by using the catalyst, which comprises the following steps: under the catalytic condition of the catalyst, mixing raw material microalgal powder with water for hydrothermal liquefaction to obtain the biomass oil.
In the above method, the amount of the catalyst may be 5% to 20%, specifically 10%, of the microalgal flour.
In the above method, the mass ratio of the microalgal flour to water may be 1: (3-5), specifically 1: 4.
in the above method, the hydrothermal liquefaction temperature may be 240 to 330 ℃, specifically 270 ℃, and the time may be 20 to 150min, specifically 30 min.
The invention has the following beneficial effects:
the catalyst prepared by the method of the invention can carry out hydrothermal liquefaction reaction on the raw material microalgae powder, and the product oil quality is obviously improved, and the catalytic effect is better. The catalyst for catalyzing and liquefying the biomass oil provided by the invention has the advantages of relieving reaction conditions and improving the yield of product oil in the reaction of preparing the biomass oil by the hydrothermal liquefaction of microalgae, and the heat value of the biomass oil is averagely 31.67MJ/kg and is relatively stable.
Drawings
FIG. 1 is a flow chart of hydrothermal liquefaction catalysis of microalgae powder.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The titanium dioxide powders in the following examples were all purchased as analytical pure titanium dioxide powders unless otherwise specified.
Example 1 preparation of a catalyst for catalytic liquefaction of Biomass oil
The catalyst was prepared as follows:
1) 36g of titanium dioxide powder is weighed, 45mL of 5 wt% nitric acid solution is added, and the titanium dioxide is acidified by shaking at the speed of 120r/s for 24 h.
2) Weighing 46.06g of nickel chloride hexahydrate, adding the nickel chloride hexahydrate into the mixed system in the step 1), then adding 45mL of deionized water (or directly adding a nickel chloride solution with the mass volume concentration of 0.36g/mL prepared by 46.06g of nickel chloride hexahydrate and 45mL of deionized water), and oscillating the mixture for 24 hours at the speed of 120r/s to obtain a solid-liquid mixture I.
3) Adding 45mL of neodymium nitrate solution with the concentration of 1.00mol/L into the solid-liquid mixture I obtained in the step 2), and oscillating for 24h at the speed of 120r/s to obtain a solid-liquid mixture II.
4) Placing the solid-liquid mixture II in a crucible, standing for 10min, removing a supernatant, and placing a precipitate in an oven to be dried for 8 hours at the temperature of 115 ℃; and (3) placing the dried solid in a muffle furnace, and roasting at 675 ℃ for 4h to obtain the catalyst, wherein the yield is 62.7 g.
Example 2 preparation of a catalyst for catalytic liquefaction of Biomass oil (different calcination temperatures)
A catalyst was prepared by following the procedure in example 1 while replacing only the calcination temperature in step 4) with 600 ℃ to obtain a catalyst yield of 55.11 g.
Example 3 preparation of a catalyst for catalytic liquefaction of Biomass oil (different calcination temperatures)
A catalyst was prepared by following the procedure of example 1 while replacing only the calcination temperature in step 4) with 800 ℃ to give a catalyst yield of 66.12 g.
Example 4 preparation of a catalyst for catalytic liquefaction of Biomass oil (different Neodymium nitrate concentrations)
A catalyst was prepared by following the procedure of example 1 while replacing only the molar concentration of neodymium nitrate in step 3) with 0.5mol/L, and the yield of the catalyst was 50.95 g.
Example 5 preparation of a catalyst for catalytic liquefaction of Biomass oil (different Neodymium nitrate concentrations)
A catalyst was prepared by following the procedure of example 1 while replacing only the molar concentration of neodymium nitrate in step 3) with 1.5mol/L, and the yield of the catalyst was 57.75 g.
Example 6 preparation of a catalyst for catalytic liquefaction of Biomass oil (different calcination times)
The catalyst was prepared by following the procedure of example 1, replacing only the calcination time in step 4) with 3 hours, and the yield of the obtained catalyst was 51.76 g.
Example 7 preparation of a catalyst for catalytic liquefaction of Biomass oil (different calcination times)
The catalyst was prepared by following the procedure of example 1, replacing only the calcination time in step 4) with 5 hours, and the yield of the obtained catalyst was 60.89 g.
Example 8 preparation of a catalyst for catalytic liquefaction of Biomass oil (different impregnation times of Neodymium nitrate solution)
The catalyst was prepared according to the procedure in example 1, replacing only the immersion time in the neodymium nitrate solution by 12h, with the following specific steps:
(1) 36g of titanium dioxide powder is weighed, 45mL of 5 wt% nitric acid solution is added, and the titanium dioxide is acidified by shaking at the speed of 120r/s for 24 h.
(2) Weighing 46.06g of nickel chloride hexahydrate, adding the nickel chloride hexahydrate into the mixed system in the step 1), then adding 45mL of deionized water (or directly adding a nickel chloride solution with the mass volume concentration of 0.36g/mL prepared by 46.06g of nickel chloride hexahydrate and 45mL of deionized water), and oscillating the mixture for 24 hours at the speed of 120r/s to obtain a solid-liquid mixture I.
(3) Adding 45mL of neodymium nitrate solution with the concentration of 1.00mol/L into the solid-liquid mixture I obtained in the step 2), and oscillating for 12h at the speed of 120r/s to obtain a solid-liquid mixture II.
(4) Placing the solid-liquid mixture II in a crucible, standing for 10min, removing a supernatant, and placing a precipitate in an oven to be dried for 8 hours at the temperature of 115 ℃; and (3) placing the dried solid in a muffle furnace, and roasting at 800 ℃ for 4h to obtain the catalyst, wherein the yield is 46.67 g.
Example 9 preparation of a catalyst for catalytic liquefaction of Biomass oil (different impregnation times of Neodymium nitrate solution)
The catalyst was prepared according to the procedure in example 3, replacing only the immersion time in the neodymium nitrate solution by 72h, with the following specific steps:
1) 36g of titanium dioxide powder is weighed, 45mL of 5 wt% nitric acid solution is added, and the titanium dioxide is acidified by shaking at the speed of 120r/s for 24 h.
2) Weighing 46.06g of nickel chloride hexahydrate, adding the nickel chloride hexahydrate into the mixed system in the step 1), then adding 45mL of deionized water (or directly adding a nickel chloride solution with the mass volume concentration of 0.36g/mL prepared by 46.06g of nickel chloride hexahydrate and 45mL of deionized water), and oscillating the mixture for 24 hours at the speed of 120r/s to obtain a solid-liquid mixture I.
3) Adding 45mL of neodymium nitrate solution with the concentration of 1.00mol/L into the solid-liquid mixture I obtained in the step 2), and oscillating for 72h at the speed of 120r/s to obtain a solid-liquid mixture II.
4) Placing the solid-liquid mixture II in a crucible, standing for 10min, removing a supernatant, and placing a precipitate in an oven to be dried for 8 hours at the temperature of 115 ℃; and (3) placing the dried solid in a muffle furnace, and roasting at 800 ℃ for 4h to obtain the catalyst, wherein the yield is 58.02 g.
Comparative example 1 preparation of non-negative Neodymium catalyst
The catalyst was prepared as follows:
1) 36g of titanium dioxide powder is weighed, 45mL of 5 wt% nitric acid solution is added, and the titanium dioxide is acidified by shaking at the speed of 120r/s for 24 h.
2) Weighing 46.06g of nickel chloride hexahydrate, adding the nickel chloride hexahydrate into the mixed system obtained in the step 1), and then adding 45mL of deionized water to soak for 24 hours (or directly adding a nickel chloride solution with the mass volume concentration of 0.36g/mL prepared by 46.06g of nickel chloride hexahydrate and 45mL of deionized water), thereby obtaining a solid-liquid mixture.
3) Placing the solid-liquid mixture in a crucible, standing for 10min, discarding the supernatant, and placing the precipitate in an oven to dry at 115 ℃; and (3) putting the dried solid in a muffle furnace, and burning for 4h at the temperature of 800 ℃ to obtain the catalyst.
Example 10 preparation of biological oil by catalytic liquefaction
The tests were conducted in a 2L batch high pressure stirred tank reactor (Parr Instruments co. 120g of dry algae powder is weighed and placed in a reaction kettle, 480mL of water is added, the catalysts prepared in the example 3 and the comparative example 1 with the content of 10 percent of the mass of the raw materials are respectively added, nitrogen is introduced to drive air, and the mixture is stirred until the mixture is uniformly mixed. The temperature of the whole reaction is controlled by a PID controller, the rotating speed knob is adjusted to 200 r/min, the temperature in the reaction kettle is heated to 270 ℃, the temperature is controlled and maintained for 30min of residence time, the heating is stopped, and the reaction kettle is cooled. And opening the reaction kettle after the reaction kettle is cooled to room temperature, standing and layering the cooled mixed solution, then carrying out primary separation, and dehydrating to obtain the viscous biomass oil. The specific process is shown in figure 1.
Elemental composition analysis of the bio-oil was determined using a vario MACRO CHNS elemental analyzer. The heat value calculation adopts a heat value calculation formula provided by Channiwala and Parikh (2002):
HHV＝0.3491×C+1.1783×H+0.1005×S－0.1034×O－0.0151×N－0.0211×A
wherein C, H, S, O, N, A represents the mass percentage of C element, H element, S element, O element, N element and ash in the biomass oil respectively.
Definition of biomass oil yield and liquefaction rate:
the liquefaction rate is (1-solid residual mass/raw material mass) × 100%;
the oil yield is (biomass oil mass/raw material mass) × 100%.
Wherein the residual mass of the solid is the mass of insoluble solid residual substances left after standing, layering and suction filtration, and is ash and catalyst residues in the microalgae raw material; the mass of the raw material is the mass of the raw material microalgae added into the reaction kettle; the biomass oil is a viscous liquid which is insoluble in water but soluble in an organic solvent after being subjected to layered suction filtration.
The product oil yields and qualities under different catalyst conditions are shown in table 1:
TABLE 1 product oil yield and quality under different catalyst conditions
As can be seen from Table 1, the catalyst prepared by the method of the present invention can significantly improve the yield of the bio-oil compared to the bio-oil prepared by adding no catalyst and adding only nickel-negative catalyst, and the carbon content and the sulfur content are reduced compared to the bio-oil prepared by adding no catalyst.
Claims (3)
1. A method for preparing biomass oil by using a catalyst comprises the following steps: under the catalytic condition of the catalyst, mixing raw material microalgal powder with water for hydrothermal liquefaction to obtain the biomass oil;
the catalyst is prepared by the method comprising the following steps:
1) mixing a nickel salt solution with titanium dioxide powder, and oscillating to obtain a solid-liquid mixture I;
2) adding a neodymium salt solution into the solid-liquid mixture I in the step 1), and oscillating to obtain a solid-liquid mixture II;
3) standing the solid-liquid mixture II obtained in the step 2), taking the precipitate, and drying and roasting to obtain the catalyst;
the method also comprises the step of acidifying the titanium dioxide powder before the step 1), specifically, adding acid into the titanium dioxide powder, and oscillating to obtain a mixed system;
in the step 1), the mass-to-volume ratio of the titanium dioxide powder to the nickel salt solution is 1 g: (1-1.5) mL; the nickel salt in the nickel salt solution is nickel chloride; the mass concentration of the nickel salt solution is 0.24-0.48 g/mL; the oscillation time is 12-36 hours;
in the step 2), the mass-to-volume ratio of the titanium dioxide powder to the neodymium salt solution is 1 g: (0.75-3.75) mL; the neodymium salt in the neodymium salt solution is neodymium nitrate; the molar concentration of the neodymium salt solution is 1.00-2.00 mol/L; the oscillation time is 24-72 hours;
in the step 3), the drying temperature is 105-115 ℃, and the drying time is 4-12 hours; the roasting temperature is 600-800 ℃, and the roasting time is 3-5 hours.
2. The method of claim 1, wherein: the addition amount of the catalyst is 5% -20% of the microalgae powder; the mass ratio of the microalgal flour to water is 1: (3-5); the temperature of the hydrothermal liquefaction is 240-330 ℃, and the time is 20-150 min.
3. The method according to claim 1 or 2, characterized in that: the acid is nitric acid; the acid is added in the form of an aqueous acid solution; adding 30-60 mL of the acid aqueous solution into every 36g of the titanium dioxide powder; the mass percentage of the acid water solution is 3% -10%; the acidification time is 12-36 hours.
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| CN108671928B (en) * | 2018-05-04 | 2021-05-18 | 中国人民大学 | Catalyst for microalgae hydrothermal liquefaction and deoxidation and preparation method and application thereof |
| CN110449158A (en) * | 2018-05-08 | 2019-11-15 | 中国人民大学 | A kind of catalyst and the preparation method and application thereof for sludge hydrothermal liquefaction deoxidation |
| CN115197736B (en) * | 2022-08-02 | 2023-08-29 | 中国矿业大学 | Method for regulating and controlling quality of supercritical hydrothermal liquefied oil of plastic garbage |
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