CN113061454A - Method for preparing bio-oil by treating waste mask through microalgae - Google Patents
Method for preparing bio-oil by treating waste mask through microalgae Download PDFInfo
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Abstract
The invention discloses a method for preparing bio-oil by treating a waste mask with microalgae, which comprises the following steps: crushing the waste mask, mixing the crushed waste mask with microalgae organisms, carrying out hydrothermal liquefaction reaction, carrying out solid-liquid separation on a reaction product, and carrying out centrifugal treatment on a mixed liquid phase to obtain the bio-oil. When the CO-HTL reaction is carried out, the mutual synergistic effect between the mixed mask and the microalgae biomass improves the quality of the bio-oil compared with that of the microalgae used as a raw material alone, improves the bio-oil yield compared with that of the recyclable waste mask used alone, effectively solves the problem that the waste mask pollutes the environment, and improves the resource utilization rate.
Description
Technical Field
The invention relates to the technical field of biomass fuel production and preparation and environmental protection, in particular to a method for preparing bio-oil by treating a waste mask through microalgae.
Background
Biological energy is a renewable energy source with wide sources, and the production and utilization of the biological energy not only help to relieve the earthThe harm and influence caused by the increasingly exhausted fossil fuel can also be reduced, and the main greenhouse gas CO can also be reduced2And the emission of nitrogen oxide and sulfur oxide gases, and air purification. In recent years, bioenergy technology has been widely used, in which microalgae can be an important source of biofuel. Among many biofuels, microalgae can be CO-hydrothermally liquefied (CO-HTL) at relatively low temperatures to obtain bio-oils. Although the bio-oil produced by using the microalgae is an excellent renewable new energy source, the bio-oil contains a large amount of protein and lipid, the content of the produced nitrogen-containing compounds and sulfur-containing compounds is high, the quality of the obtained bio-oil is not high, and the bio-oil has certain pollution to the environment.
The conversion of the plastic waste into the bio-oil has high quality, but the bio-oil can be carried out at very high temperature, the energy consumption is high, and the yield of the obtained bio-oil is low.
Disclosure of Invention
The invention aims to provide a method for preparing bio-oil by treating a waste mask through microalgae, which can solve the pollution problem of the waste mask and improve the quality and the yield of the bio-oil at a relatively low temperature.
In order to achieve the above object, the present invention provides a method for preparing bio-oil by treating a waste mask with microalgae, comprising the steps of: crushing the waste mask, mixing the crushed waste mask with microalgae organisms, carrying out hydrothermal liquefaction reaction, carrying out solid-liquid separation on a reaction product, and centrifuging a mixed liquid phase to obtain bio-oil; wherein, the hydrothermal liquefaction reaction comprises the following specific processes: mixing the mixture of the waste mask and the microalgae organisms with an organic solvent according to the mass-volume ratio of 1-2g:9mL, putting the mixture into a reaction kettle, and reacting for 30-60min under the conditions that the reaction temperature is 280-320 ℃, the pressure is 3.0-5.0MPa and the stirring speed is 450-550 rpm; wherein the organic solvent is ethanol solvent with volume fraction of 50%. .
The beneficial effect who adopts above-mentioned scheme is: microalgae can be used for photosynthesis to fix C elements in the atmosphere, and microalgae can synthesize oil by using substances of microalgae, so that oil can be produced by using microalgae, and in addition, a small amount of C is contained in the waste mask, and the oil can still be produced under the action of 300 ℃ at a high temperature when HTL reaction is carried out. Meanwhile, because microalgae organisms contain a large amount of nitrogen and sulfur elements, a large amount of sulfur and nitrogen compounds can be generated to pollute the air in the process of producing the bio-oil, and the waste mask greatly improves the quality of the bio-oil and effectively improves the yield of the bio-oil by utilizing the synergistic effect of the waste mask and the microalgae biomass, and simultaneously reduces the pollution of the mask to the environment. The concentrated algae stock solution can be converted into the biological crude oil in a short time under a high-pressure environment through a hydrothermal liquefaction reaction, and the added waste mask can increase the carbon-oxygen content and reduce the nitrogen-sulfur content, so that the prepared biological crude oil has better quality and less pollution of sulfur-nitrogen compounds.
Furthermore, the crushing degree of the waste mask is 1-4mm, and the microalgae organisms are spirulina platensis.
The beneficial effect who adopts above-mentioned scheme is: spirulina platensis can convert carbonic acid and solar energy in living environment into saccharides and other nutrients to nourish itself, and has higher growth, division and proliferation speed than many organisms performing photosynthesis, so that it has better quality and efficiency in preparing biofuel, etc.
Furthermore, the mixing mass ratio of the waste mask to the microalgae organisms is 3: 1-9.
Further, the mixing mass ratio of the waste mask to the microalgae organisms is 1: 3.
Further, still include: and (3) placing microalgae strains in a photocatalytic reactor containing wastewater for amplification culture, and then harvesting and drying the microalgae after the exponential growth stage is finished, and mixing the microalgae with the crushed waste mask.
The beneficial effect who adopts above-mentioned scheme is: at the moment, the microalgae organisms are in the best growth cycle, the viability, the cell activity and the like of the microalgae organisms are in the best states, the propagation is fast, the adaptability is strong, and the effect of the microalgae organisms for preparing the bio-oil is better.
Further, the hydrothermal liquefaction reaction comprises the following specific steps: mixing a mixture of the waste mask and microalgae organisms with an organic solvent according to the mass-volume ratio of 1g to 9mL, putting the mixture into a reaction kettle, and reacting for 45min under the conditions that the reaction temperature is 300 ℃, the pressure is 4.0MPa and the stirring speed is 500 rpm; wherein the organic solvent is ethanol solvent with volume fraction of 50%.
Further, the solid-liquid separation process is to use a filter membrane with the aperture of 0.4-0.5 μm to carry out solid-liquid separation, and the solid product obtained by separation is biochar.
Further, the specific process of the centrifugal treatment is as follows: and (3) putting the mixed liquid phase generated by solid-liquid separation into an organic solvent, centrifuging for 1-3min under the condition that the centrifugal force is 200 Xg to obtain two liquid phases, separating, and evaporating the separated lower liquid phase for 20-24h under the condition of 55-65 ℃ to obtain the bio-oil.
The beneficial effect who adopts above-mentioned scheme is: the mixed liquid phase generated by solid-liquid separation is the mixed phase of solvent dichloromethane, water and solute biological oil, the water and dichloromethane-biological oil phase can be separated by centrifugation, the dichloromethane-biological oil phase is evaporated, and dichloromethane can be evaporated by different boiling points to prepare the biological oil with higher purity.
Further, the organic solvent in the centrifugation process is dichloromethane.
The beneficial effect who adopts above-mentioned scheme is: the boiling point of the dichloromethane is low, and the dichloromethane can be evaporated at a low temperature in an oven to prepare the bio-oil without damaging the quality of the bio-oil.
In summary, the invention has the following advantages:
1. the invention can effectively solve the problem of environmental pollution caused by that the mask is discarded everywhere and cannot be degraded, reduces the harm to the environment and people, can be used for centralized treatment of the disposable mask and has environmental protection effect;
2. when the CO-HTL reaction is carried out, the mutual synergistic effect between the mixed mask and the microalgae biomass improves the quality of the bio-oil compared with the method of singly using the microalgae as a raw material, and improves the yield of the bio-oil compared with the method of singly using the recyclable waste mask;
3. in the invention, the microalgae contains a large amount of proteins and lipids, and peptide bonds and a small amount of disulfide bonds of the proteins and lipids cause nitrogen-containing compounds and sulfur-containing compounds generated when the element N, S in the microalgae is pyrolyzed to pollute the environment; the mask does not contain N, S element, but the pyrolysis of the mask requires high temperature and long time, when the mask and the mask are mixed according to a certain proportion, the content of the generated nitrogen-containing compound and sulfur-containing compound is obviously reduced, the problem of environmental pollution is reduced, and in addition, the waste of energy is also reduced.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a graph showing the contents of various products prepared by examples 1 to 3 and comparative examples 1 to 2;
wherein, A, biological oil; B. biochar; C. water-soluble compounds and gases;
FIG. 3 is a graph showing the contents of various compounds in bio-oils prepared by examples 1 to 3 and comparative examples 1 to 2;
wherein, a, carboxylic acid/carboxylate; b. alkanes/alkenes; c. a phenolic compound; d. aromatic hydrocarbons; e. a nitrogen-containing compound; f. an oxygen-containing compound; g. and (c) other substances.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
As shown in fig. 1, the present embodiment provides a method for preparing bio-oil by treating a waste mask with microalgae, comprising the following steps:
(1) culturing Spirulina platensis in a photocatalytic reactor filled with wastewater, drying and storing after exponential growth stage is finished, and selecting and weighing 1.5g of dried Spirulina platensis and 0.5g of waste gauze mask particles, crushing with a crusher, and mixing well, wherein the particle diameter of the waste gauze mask particles is 0.4 mm;
(2) mixing the product mixed in the step (1) with water, adding 18mL of 50% ethanol solution by volume fraction, putting the mixture into a miniature magnetic stirring high-pressure hydrogenation reaction kettle together, stirring and reacting for 45min under the conditions that the temperature is 300 ℃, the rotating speed is 500rpm and the pressure is 3.5MPa, and cooling to room temperature;
(3) taking out the product in the reaction kettle, performing solid-liquid separation by using a filter membrane of 0.45 mu m, drying the solid obtained by separation to prepare biochar, wherein the liquid phase after separation is a mixed solution;
(4) mixing the mixed solution with dichloromethane, placing into a centrifuge, centrifuging for 2min under the condition of centrifugal force of 200 Xg, centrifuging to obtain upper layer water and lower layer biological oil and dichloromethane mixed phase, separating the lower layer solution, and evaporating in an oven at 60 deg.C for 24 hr to obtain biological oil.
The bio-oil obtained in example 1 was weighed and its yield was calculated according to the following formula.
Bio-oil yield (Y)oil,％)＝(M1/M0)×100；
Biochar yield (Y)char,％)＝(M2/M0)×100；
Gas yield (WSG) (%) 100- (Y)oil+Ychar)；
Wherein M is0Is the total mass of the biomass, M1Is the quality of the bio-oil, M2The result is shown in figure 2, and the yield of bio-oil is 21.99 percent, which is the quality of the bio-carbon.
Example 2
The embodiment provides a method for preparing bio-oil by using microalgae to treat a waste mask, which comprises the following steps:
(1) culturing Spirulina platensis in a photocatalytic reactor filled with wastewater, drying and storing after the exponential growth stage is finished, and selecting and weighing 1g of dried Spirulina platensis and 1g of waste mask particles until a crusher is broken and uniformly mixed, wherein the particle diameter of the waste mask particles is 0.4 mm;
(2) mixing the product mixed in the step (1) with water, adding 18mL of 50% ethanol solution by volume fraction, putting the mixture into a miniature magnetic stirring high-pressure hydrogenation reaction kettle together, stirring and reacting for 45min under the conditions that the temperature is 300 ℃, the rotating speed is 500rpm and the pressure is 3.5MPa, and cooling to room temperature;
(3) taking out the product in the reaction kettle, performing solid-liquid separation by using a filter membrane of 0.45 mu m, drying the solid obtained by separation to prepare biochar, wherein the liquid phase after separation is a mixed solution;
(4) mixing the mixed solution with dichloromethane, placing into a centrifuge, centrifuging for 2min under the condition of centrifugal force of 200 Xg, centrifuging to obtain upper layer water and lower layer biological oil and dichloromethane mixed phase, separating the lower layer solution, and evaporating in an oven at 60 deg.C for 24 hr to obtain biological oil.
The bio-oil obtained in example 2 was weighed and the yield thereof was calculated according to the formula of example 1, and as a result, as shown in fig. 2, the yield of bio-oil was 17.84%.
Example 3
The embodiment provides a method for preparing bio-oil by using microalgae to treat a waste mask, which comprises the following steps:
(1) culturing Spirulina platensis in a photocatalytic reactor filled with wastewater, drying and storing after exponential growth stage is finished, and selecting and weighing 0.5g of dried Spirulina platensis and 1.5g of waste gauze mask particles, crushing with a crusher, and mixing well, wherein the particle diameter of the waste gauze mask particles is 0.4 mm;
(2) mixing the product mixed in the step (1) with water, adding 18mL of 50% ethanol solution by volume fraction, putting the mixture into a miniature magnetic stirring high-pressure hydrogenation reaction kettle together, stirring and reacting for 45min under the conditions that the temperature is 300 ℃, the rotating speed is 500rpm and the pressure is 3.5MPa, and cooling to room temperature;
(3) taking out the product in the reaction kettle, performing solid-liquid separation by using a filter membrane of 0.45 mu m, drying the solid obtained by separation to prepare biochar, wherein the liquid phase after separation is a mixed solution;
(4) mixing the mixed solution with dichloromethane, placing into a centrifuge, centrifuging for 2min under the condition of centrifugal force of 200 Xg, centrifuging to obtain upper layer water and lower layer biological oil and dichloromethane mixed phase, separating the lower layer solution, and evaporating in an oven at 60 deg.C for 24 hr to obtain biological oil.
The bio-oil obtained in example 3 was weighed and the yield thereof was calculated according to the formula of example 1. As a result, as shown in FIG. 2, the yield of bio-oil was 10.12%.
Comparative example 1
The embodiment provides a method for preparing bio-oil by using microalgae, which comprises the following steps:
(1) culturing Spirulina platensis in a photocatalytic reactor filled with wastewater, drying and storing after the exponential growth stage is finished, and selecting and weighing 2.0g of dried Spirulina platensis, crushing with a crusher, and mixing well;
(2) mixing the product obtained in the step (1) with water, adding 18mL of 50% ethanol solution by volume fraction, putting the mixture into a miniature magnetic stirring high-pressure hydrogenation reaction kettle together, stirring and reacting for 45min under the conditions that the temperature is 300 ℃, the rotating speed is 500rpm and the pressure is 3.5MPa, and cooling to room temperature;
(3) taking out the product in the reaction kettle, performing solid-liquid separation by using a filter membrane of 0.45 mu m, drying the solid obtained by separation to prepare biochar, wherein the liquid phase after separation is a mixed solution;
(4) mixing the mixed solution with dichloromethane, placing into a centrifuge, centrifuging for 2min under the condition of centrifugal force of 200 Xg to obtain upper layer water and lower layer biological oil and dichloromethane mixed phase, separating the lower layer solution, and evaporating in an oven at 60 deg.C for 24 hr to obtain biological oil with yield of 24.12%.
Comparative example 2
The embodiment provides a method for preparing bio-oil by using a waste mask, which comprises the following steps:
(1) weighing 2.0g of waste mask until the waste mask is smashed by a smashing machine and uniformly mixed;
(2) mixing the product obtained in the step (1) with water, adding 18mL of 50% ethanol solution by volume fraction, putting the mixture into a miniature magnetic stirring high-pressure hydrogenation reaction kettle together, stirring and reacting for 45min under the conditions that the temperature is 300 ℃, the rotating speed is 500rpm and the pressure is 3.5MPa, and cooling to room temperature;
(3) taking out the product in the reaction kettle, performing solid-liquid separation by using a filter membrane of 0.45 mu m, drying the solid obtained by separation to prepare biochar, wherein the liquid phase after separation is a mixed solution;
(4) mixing the mixed solution with dichloromethane, placing into a centrifuge, centrifuging for 2min under the condition of centrifugal force of 200 Xg to obtain upper layer water and lower layer biological oil and dichloromethane mixed phase, separating the lower layer solution, and evaporating in an oven at 60 deg.C for 24 hr to obtain biological oil with yield of 17.46%.
The bio-oil and bio-char obtained in comparative example 1 and comparative example 2 were calculated according to the formulas described in examples 1 to 3, and the results are shown in FIG. 2.
The elemental analysis of the mixture crushed by the crusher in examples 1 to 3 and comparative examples 1 to 2 was carried out, and the analysis results are shown in Table 1.
TABLE 1 analysis table of element content in mixture of different mixing ratios
| Detailed Description | Nitrogen (%) | Carbon (%) | Hydrogen (%) | Sulfur (%) | Oxygen (%) |
| Comparative example 1 | 9.13 | 42.19 | 5.88 | 0.72 | 28.49 |
| Example 1 | 3.16 | 70.71 | 11.45 | 0.34 | 28.04 |
| Example 2 | 1.91 | 75.53 | 12.18 | 0.13 | 17.05 |
| Example 3 | 0.37 | 82.75 | 12.13 | 0 | 1.53 |
| Comparative example 2 | 0 | 83.84 | 13.77 | 0 | 0.64 |
As can be seen from table 1, the nitrogen and sulfur contents in comparative example 1 and example 1 are high, and NOx and SOx are generated in a large amount by hydrothermal liquefaction reaction, and the discharged air is harmful to human bodies and animal and plant organisms. Therefore, the proportion of microalgae organisms is not high enough in the process of producing bio-oil by mixing. Comparative example 2 shows that it does not contain microalgae organism, and its broken product contains no nitrogen and sulfur elements and contains high content of carbon elements, so its bio-oil yield is low. As can be seen from fig. 2, the bio-oil yield is higher as the proportion of microalgae organisms in the mixture is higher, and as can be seen from fig. 3, when only microalgae organisms are contained, the content of nitrogen-containing compounds is highest, which seriously affects the environment and the quality of bio-oil, and the content of carboxylic acid/carboxylic ester is also kept at a common concentration, the proportion of microalgae organisms and waste masks is not optional; when the raw material only contains the mask, the bio-oil yield is very low, but the quality of the bio-oil is higher than that of the microalgae biomass. Therefore, the mask and the microalgae biomass in different proportions are subjected to hydrothermal liquefaction together, and the mask and the microalgae biomass can generate a synergistic effect, so that the quality of the bio-oil is better than that of the bio-oil under the condition of only microalgae biomass. As can be seen from fig. 2, when the mass ratio of the microalgae biomass to the mask is 3:1, the comprehensive aspects are better. Therefore, the biological oil is prepared by selecting the mass ratio of microalgae organisms to the waste mask to be 3:1, the generation of greenhouse gases can be reduced, and the yield and the quality of the biological oil are improved.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (8)
1. A method for improving the yield of bio-oil by using microalgae to treat a waste mask is characterized by comprising the following steps:
crushing the waste mask, mixing the crushed waste mask with microalgae organisms, carrying out hydrothermal liquefaction reaction, carrying out solid-liquid separation on a reaction product, and centrifuging a mixed liquid phase to obtain bio-oil;
wherein the hydrothermal liquefaction reaction comprises the following specific steps: mixing the mixture of the waste mask and the microalgae organisms with an organic solvent according to the mass-volume ratio of 1-2g:9mL, putting the mixture into a reaction kettle, and reacting for 30-60min under the conditions that the reaction temperature is 280-320 ℃, the pressure is 3.0-5.0MPa and the stirring speed is 450-550 rpm; wherein the organic solvent is ethanol solvent with volume fraction of 50%.
2. The method for preparing bio-oil using microalgae to treat the waste masks as set forth in claim 1, wherein: the diameter of the crushed waste mask is 1-4mm, and the microalgae organisms are Spirulina platensis.
3. The method for preparing bio-oil using microalgae to treat the waste masks as set forth in claim 1 or 2, wherein: the mixing mass ratio of the waste mask to the microalgae organisms is 3: 1-9.
4. The method for preparing bio-oil by using microalgae to treat waste masks as claimed in claim 1 or 2, further comprising: and (3) placing microalgae strains in a photocatalytic reactor containing wastewater for amplification culture, and then harvesting and drying the microalgae after the exponential growth stage is finished, and mixing the microalgae with the crushed waste mask.
5. The method for preparing bio-oil by using microalgae to treat waste masks as claimed in claim 1, wherein the hydrothermal liquefaction reaction comprises the following specific steps: mixing a mixture of the waste mask and microalgae organisms with an organic solvent according to the mass-volume ratio of 1g to 9mL, putting the mixture into a reaction kettle, and reacting for 45min under the conditions that the reaction temperature is 300 ℃, the pressure is 4.0MPa and the stirring speed is 500 rpm; wherein the organic solvent is ethanol solvent with volume fraction of 50%.
6. The method for preparing bio-oil using microalgae to treat the waste masks as set forth in claim 1, wherein: the specific process of the solid-liquid separation is to use a filter membrane with the aperture of 0.4-0.5 mu m to carry out the solid-liquid separation, and the solid product obtained by the separation is the biochar.
7. The method for preparing bio-oil by using microalgae to treat waste masks as claimed in claim 1, wherein the centrifugation comprises the following specific steps: and (3) putting the mixed liquid phase generated by solid-liquid separation into an organic solvent, centrifuging for 1-3min under the condition that the centrifugal force is 200 Xg to obtain two liquid phases, separating, and evaporating the separated lower liquid phase for 20-24h under the condition of 55-65 ℃ to obtain the bio-oil.
8. The method for preparing bio-oil using microalgae to treat the waste masks as set forth in claim 7, wherein: the organic solvent in the centrifugation process is dichloromethane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113801725A (en) * | 2021-09-18 | 2021-12-17 | 华中科技大学 | Biofuel and preparation method and application thereof |
| KR20230076145A (en) * | 2021-11-22 | 2023-05-31 | 한국에너지기술연구원 | A waste mask gasfication system |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113801725A (en) * | 2021-09-18 | 2021-12-17 | 华中科技大学 | Biofuel and preparation method and application thereof |
| KR20230076145A (en) * | 2021-11-22 | 2023-05-31 | 한국에너지기술연구원 | A waste mask gasfication system |
| KR102564465B1 (en) | 2021-11-22 | 2023-08-09 | 한국에너지기술연구원 | A waste mask gasfication system |
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Application publication date: 20210702 |