CN112899067A - Method for increasing sugar content in biological oil - Google Patents
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- CN112899067A CN112899067A CN202110048372.1A CN202110048372A CN112899067A CN 112899067 A CN112899067 A CN 112899067A CN 202110048372 A CN202110048372 A CN 202110048372A CN 112899067 A CN112899067 A CN 112899067A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
Abstract
The invention discloses a method for improving sugar content in biological oil, which comprises the following steps: mixing the biomass material with an acid solution, stirring at the temperature of less than or equal to 70 ℃, standing, carrying out acid pickling pretreatment on the biomass material, carrying out solid-liquid separation, washing, and drying to obtain an acid-pickled biomass material; and carrying out pyrolysis treatment on the acid-washed biomass material to obtain the bio-oil with high sugar content. According to the method, the yield and the sugar content of the bio-oil are improved by carrying out the pyrolysis treatment after the acid washing pretreatment, wherein the sugar content is improved from 2.8% to 51.52%, and the yield is improved from 24.74 wt.% to 30.18 wt.%, so that the defects of low yield, low sugar content and the like of the bio-oil in the conventional pyrolysis method are overcome, and the method has the advantages of simple process, convenience in operation, mild conditions and the like, is suitable for large-scale preparation of high-quality bio-oil, and has very important significance for improving the quality of the bio-oil and promoting the resource utilization efficiency of biomass materials.
Description
Technical Field
The invention belongs to the field of liquid fuels, relates to a method for improving sugar content in bio-oil, and particularly relates to a method for improving sugar content in bio-oil by utilizing acid washing pretreatment.
Background
With the continuous advance of urbanization and the improvement of the living standard of people, the consumption of energy sources is gradually increased year by year around the world. However, in the world energy industry today, traditional fossil fuels remain the main source of energy, and the environmental problems associated with the reduction of traditional fossil fuel reserves and fuel usage are becoming increasingly non-negligible, and the production of sustainable, renewable alternative energy has become an inevitable global problem. The biomass waste is rich in organic matter and has a huge reserve, and therefore the biomass waste enters the field of researchers. From the waste treatment perspective, an effective and reasonable energy conversion technology is developed, so that the biomass waste can be used as a raw material to produce chemicals to be used as an energy donor to replace the traditional fuel, an effective way is provided for the treatment of the biomass waste, and the problem of energy utilization can be solved.
Most biomass waste is a biocomposite material composed of cellulose, hemicellulose and lignin, wherein depolymerization and conversion of cellulose and hemicellulose are key issues for energy utilization of biomass materials. Through a certain method, the biological oil is cracked and converted into the biological oil which can be further utilized, and the saccharides in the biological oil have high market price and are important multifunctional products for producing high value-added chemicals and pharmaceutical additives. For example, fermentable sugars can be utilized by microorganisms to produce alcohol. At present, a common method for recovering organic matters from biomass is enzyme hydrolysis, in which cellulose and hemicellulose are hydrolyzed by adding biological enzyme to obtain biological oil with rich sugar content, however, the method has slow hydrolysis rate, and usually requires adding a plurality of enzymes for mixing, resulting in high cost, and the defects are not favorable for the development of the technology.
The pyrolysis technology is a new technology for recycling organic matters from biomass wastes for energy utilization, the capital cost of the pyrolysis technology is lower than that of a biochemical approach, the operation process is simpler, and the biomass can be rapidly and fully decomposed at 550 ℃ without using enzymes or catalysts to obtain solid products (biochar), liquid products (bio-oil) and gas products (non-condensable gas). However, the bio-oil component obtained by direct pyrolysis of biomass feedstock is very complex, the amount of sugars produced by direct pyrolysis of biomass is very small compared to the theoretical yield based on a single cellulose fraction, and the raw materialFactors such as the cellulose purity, physical properties and experimental conditions of the material can influence the bio-oil component. In addition, because the alkali metals and alkaline earth metals (AAEMs) contained in the biomass have certain catalytic action, organic matters can be catalyzed to decompose and form more small molecular compounds in the pyrolysis process, so that the yield of the bio-oil is reduced, and the generation of saccharide products in the bio-oil is not facilitated. The pyrolysis technology also comprises a microwave cracking technology, for example, the biological oil is prepared by adopting a mode of steam explosion under an acidic condition and microwave pyrolysis under a microwave auxiliary agent and a catalyst, because the steam explosion is carried out under the conditions of high temperature and high pressure (the temperature is 180-200 ℃, and the pressure is 0.5-1.0MpPa), the treatment condition can change the organic component structure of the raw material, decompose some substances with low thermal stability, reduce the yield of the biological oil and reduce the sugar content in the biological oil; meanwhile, sulfur and nitrogen containing components in the acid are easy to remain in the solid when the biomass material is subjected to steam explosion, so that the content of sulfur and nitrogen in the bio-oil is easy to increase, and the clean utilization of the bio-oil is restricted; in addition, in order to increase the temperature rise rate of the biomass in the microwave pyrolysis process, not only the microwave absorption factors (water and trace elements Na) of the biomass need to be effectively utilized+And K+Etc.), microwave additives and catalysts are additionally added, but both microwave absorption factors of biomass itself and the subsequent additional microwave additives and catalysts affect the yield of the bio-oil, wherein when the biomass material is subjected to microwave pyrolysis under the above conditions, the direct pyrolysis products of cellulose, hemicellulose, lignin, etc. in the biomass are also susceptible to secondary cracking in the high-temperature and high-pressure environment of the microwave pyrolysis, so that more small-molecule substances are generated, the yield of the biogas is increased, and finally the yield of the bio-oil is low. Therefore, the method for improving the yield and the sugar content of the bio-oil, which is simple in process and convenient to operate, is obtained, and has very important significance for improving the quality of the bio-oil and effectively promoting the further development of resource utilization of biomass.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art, and provide a method for improving the sugar content in the bio-oil, which has the advantages of simple process, convenient operation and mild conditions, not only can effectively improve the sugar content in the bio-oil and improve the quality of the bio-oil, but also can improve the yield of the bio-oil, and effectively promote the further development of resource utilization of biomass.
In order to solve the technical problems, the invention adopts the technical scheme that:
a method for increasing the sugar content of a bio-oil, comprising the steps of:
s1, mixing the biomass material with an acid solution, stirring at a temperature of less than or equal to 70 ℃, standing, carrying out acid washing pretreatment on the biomass material, carrying out solid-liquid separation, washing, and drying to obtain an acid-washed biomass material;
s2, carrying out pyrolysis treatment on the acid-washed biomass material obtained in the step S1 to obtain the bio-oil with high sugar content.
In the method for increasing the sugar content in the bio-oil, the stirring is performed at a temperature of 15-50 ℃ in step S1.
In the above method for increasing the sugar content in the bio-oil, it is further improved that in step S1, the stirring time is 2h to 5 h; the standing time is 0.5-1 h.
In the above method for increasing the sugar content in the bio-oil, further improvement is that in step S1, the mass-to-volume ratio of the biomass material to the acid solution is 1 g: 10 mL; the acid solution is any one of hydrochloric acid, sulfuric acid, formic acid and acetic acid; the mass fraction of the acid solution is 1-7%.
In the above method for increasing the sugar content in the bio-oil, the acid solution is further improved in step S1, and the mass fraction of the acid solution is 3% to 4%.
In step S1, the biomass material is rice husk; the biomass material further comprises, prior to use: the biomass material is crushed to be less than or equal to 60 meshes.
In step S1, the solid-liquid separation is performed by suction filtering the acid-washed pretreatment product; the washing is to wash the solid-liquid separation product by water until the pH value of the washing liquid is 7; the drying is carried out at the temperature of 85-105 ℃; the drying time is 24-48 h.
In the method for increasing the sugar content in the bio-oil, in a further improvement, in step S2, the pyrolysis treatment is performed under the protection of nitrogen; the heating rate in the pyrolysis treatment process is 10 ℃/min; the temperature of the pyrolysis treatment is 550 ℃; the pyrolysis treatment time was 30 min.
In the above method for increasing the sugar content in the bio-oil, in a further improvement, in step S2, the pyrolysis treatment further includes the following steps: and (3) conveying a gas product generated in the pyrolysis treatment to an organic solvent by taking nitrogen or argon as a carrier gas for condensation, evaporating to remove the organic solvent in the obtained condensate, and collecting to obtain the biological oil with high sugar content.
In the method for increasing the sugar content in the bio-oil, the organic solvent is acetone; the condensation is carried out under ice-water bath conditions; the temperature of the evaporation was 57 ℃.
Compared with the prior art, the invention has the advantages that:
(1) aiming at the defects of low yield, low sugar content and the like of the bio-oil caused by alkali metal and alkaline earth metal (AAEMs) contained in the biomass material in the conventional pyrolysis method, the invention creatively provides a method for improving the sugar content in the bio-oil, the biomass material is mixed with an acid solution for acid washing pretreatment at the temperature of less than or equal to 70 ℃, so that most of the AAEMs in the biomass material are effectively removed, the adverse effect of the AAEMs on subsequent pyrolysis treatment is eliminated, the AAEMs are removed under the condition of mild temperature, the influence on the original organic components and structure of the biomass material is minimum, the loss of the biomass can be reduced to the maximum extent, more biomass can be converted into sugar after the pyrolysis treatment, and the bio-oil with high sugar content is obtained. Compared with the conventional method for directly carrying out pyrolysis treatment on the biomass material, the method disclosed by the invention has the advantages that the pyrolysis treatment is carried out after the acid washing pretreatment, so that the content of sugar in the bio-oil is improved, the yield of the bio-oil is also improved, the content of sugar in the bio-oil is improved from 2.8% to 42.13-51.52%, the yield of the bio-oil is improved from 24.74 wt.% to 27.26-30.18 wt.%, the defects of low yield of the bio-oil, low sugar content and the like in the conventional pyrolysis method are overcome, and the method has very important significance for improving the resource utilization efficiency of the biomass material. Meanwhile, compared with the conventional pyrolysis (such as acid leaching, steam explosion or microwave treatment and acid combination) method, the method disclosed by the invention can be used for obtaining the bio-oil with higher yield and sugar content, is milder in treatment conditions and lower in treatment cost, and has very important significance for preparing the bio-oil with low cost and high quality. The method for improving the sugar content in the bio-oil has the advantages of simple process, convenient operation, mild conditions and the like, is suitable for preparing high-quality bio-oil on a large scale, and is beneficial to resource utilization of biomass materials and bio-oil.
(2) In the invention, the pickling pretreatment condition is optimized, specifically stirring is carried out at the temperature of 15-50 ℃, and the product is washed until the pH value of the washing liquid is 7, wherein the temperature of the pickling pretreatment is optimized to ensure that the bio-oil contains higher sugar content on the premise of ensuring higher bio-oil yield, because if the temperature is too low, most AAEMs in the biomass material are difficult to remove, and more sugar is converted into furan at higher temperature, so that the sugar content in the bio-oil is further reduced; meanwhile, the product is thoroughly cleaned, so that chlorine or sulfur brought in the acid liquor is effectively removed, and cleaner bio-oil can be obtained.
Drawings
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
FIG. 1 is a bar graph of the yield of bio-oil obtained under different treatment conditions in examples 1 to 5 of the present invention.
FIG. 2 is a bar graph of sugar content in bio-oil obtained under different treatment conditions in examples 1 to 5 of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
In the examples of the present invention, the raw materials and instruments used were all commercially available. If not stated otherwise, the process adopted is a conventional process, the equipment adopted is conventional equipment, and the obtained data are average values of more than three repeated experiments.
Example 1
A method for increasing the sugar content of a bio-oil, comprising the steps of:
crushing rice hulls to less than 60 meshes to obtain uniform rice hulls, uniformly mixing 15g of rice hulls with 150mL of hydrochloric acid solution with the mass fraction of 3%, placing the mixture in a magnetic stirrer, stirring the mixture at 25 ℃ for 3 hours, standing the mixture of the rice hulls and the acid solution for 0.5 hour, separating the acid solution from the rice hulls by utilizing vacuum filtration, filtering the mixture by using ultrapure water, washing the obtained filtered product until the pH value of the ultrapure water is close to neutral (the pH value is 7), and continuously drying the acid-washed rice hulls in an oven with the temperature of 105 ℃ for 48 hours.
Spreading 6g of the rice hulls after acid washing in a quartz boat, placing the quartz boat in a tubular furnace reactor under the protection of nitrogen, heating the quartz boat from room temperature to pyrolysis final temperature of 550 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 30min, conveying gas products generated in the pyrolysis treatment process into acetone by taking nitrogen as carrier gas, condensing the gas products in a condensing device, collecting condensate, heating the condensate at 57 ℃, and removing the acetone through evaporation treatment to obtain the bio-oil. The components in the bio-oil are determined by gas chromatography-mass spectrometry (GC-MS), and the results show that: the yield and sugar content of the bio-oil obtained were 30.18 wt.% and 48.29%, respectively.
Example 2
A method for increasing the sugar content of a bio-oil, comprising the steps of:
crushing rice hulls to less than 60 meshes to obtain uniform rice hulls, uniformly mixing 15g of rice hulls with 150mL of sulfuric acid solution with the mass fraction of 3%, placing the mixture in a magnetic stirrer, stirring the mixture at 25 ℃ for 2 hours, standing the mixture of the rice hulls and the acid solution for 0.5 hour, separating the acid solution from the rice hulls by utilizing vacuum filtration, filtering the mixture by using ultrapure water, washing the obtained filtered product until the pH value of the ultrapure water is close to neutral (the pH value is 7), and continuously drying the acid-washed rice hulls in an oven with the temperature of 105 ℃ for 48 hours.
Spreading 6g of the rice hulls after acid washing in a quartz boat, placing the quartz boat in a tubular furnace reactor under the protection of nitrogen, heating the quartz boat from room temperature to pyrolysis final temperature of 550 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 30min, conveying gas products generated in the pyrolysis treatment process into acetone by taking nitrogen as carrier gas, condensing the gas products in a condensing device, collecting condensate, heating the condensate at 57 ℃, and removing the acetone through evaporation treatment to obtain the bio-oil. The components in the bio-oil are determined by gas chromatography-mass spectrometry (GC-MS), and the results show that: the yield and sugar content of the bio-oil obtained were 28.13 wt.% and 51.52%, respectively.
Example 3
A method for increasing the sugar content of a bio-oil, comprising the steps of:
crushing rice hulls to less than 60 meshes to obtain uniform rice hulls, uniformly mixing 15g of rice hulls with 150mL of formic acid solution with the mass fraction of 3%, placing the mixture in a magnetic stirrer, stirring the mixture at 25 ℃ for 5 hours, standing the mixture of the rice hulls and the acid solution for 0.5 hour, separating the acid solution from the rice hulls by utilizing vacuum filtration, filtering the mixture by using ultrapure water, washing the obtained filtered product until the pH value of the ultrapure water is close to neutral (the pH value is 7), and continuously drying the acid-washed rice hulls in an oven at 85 ℃ for 48 hours.
Spreading 6g of the rice hulls after acid washing in a quartz boat, placing the quartz boat in a tubular furnace reactor under the protection of nitrogen, heating the quartz boat from room temperature to pyrolysis final temperature of 550 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 30min, conveying gas products generated in the pyrolysis treatment process into acetone by taking nitrogen as carrier gas, condensing the gas products in a condensing device, collecting condensate, heating the condensate at 57 ℃, and removing the acetone through evaporation treatment to obtain the bio-oil. The components in the bio-oil are determined by gas chromatography-mass spectrometry (GC-MS), and the results show that: the yield and sugar content of the bio-oil obtained were 24.69 wt.% and 42.13%, respectively.
Example 4
A method for increasing the sugar content of a bio-oil, comprising the steps of:
crushing rice hulls to less than 60 meshes to obtain uniform rice hulls, uniformly mixing 15g of rice hulls with 150mL of 3% acetic acid solution by mass fraction, placing the mixture in a magnetic stirrer, stirring the mixture at 25 ℃ for 3 hours, standing the mixture of the rice hulls and the acid solution for 0.5 hour, separating the acid solution from the rice hulls by utilizing vacuum filtration, filtering the mixture by using ultrapure water, washing the obtained filtered product until the pH value of the ultrapure water is close to neutral (the pH value is 7), and continuously drying the acid-washed rice hulls in an oven at 105 ℃ for 24 hours.
Spreading 6g of the rice hulls after acid washing in a quartz boat, placing the quartz boat in a tubular furnace reactor under the protection of nitrogen, heating the quartz boat from room temperature to pyrolysis final temperature of 550 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 30min, conveying gas products generated in the pyrolysis treatment process into acetone by taking nitrogen as carrier gas, condensing the gas products in a condensing device, collecting condensate, heating the condensate at 57 ℃, and removing the acetone through evaporation treatment to obtain the bio-oil. The components in the bio-oil are determined by gas chromatography-mass spectrometry (GC-MS), and the results show that: the yield and sugar content of the bio-oil obtained were 27.26 wt.% and 44.61%, respectively.
Example 5
A method of increasing the sugar content of a bio-oil, substantially as in example 1, except that: the mass fractions of the hydrochloric acid solution in example 5 were 1%, 5%, and 7%.
In example 5, when the mass fractions of the hydrochloric acid solution were 1%, 5% and 7%, the yields of bio-oil were 29.7 wt.%, 28.93 wt.% and 27.72%, respectively, and the sugar contents were 36.14%, 31.76% and 30.53%, respectively.
Control group: the acid washing pretreatment was not performed, and the other conditions were the same as in example 1.
The contents of bio-oil, bio-char and biogas produced under different conditions were tested, and the results are shown in fig. 1; the sugar content of the bio-oil prepared under different conditions was also tested, and the results are shown in fig. 2. FIG. 1 is a bar graph of the yield of bio-oil obtained under different treatment conditions in examples 1 to 5 of the present invention. In fig. 1, liquid, solid and gas are all products after pyrolysis treatment, wherein liquid refers to bio-oil, solid refers to bio-carbon, and gas refers to biogas (non-condensable gas).
FIG. 2 is a bar graph of sugar content in bio-oil obtained under different treatment conditions in examples 1 to 5 of the present invention.
As can be seen from fig. 1 and 2, compared with the conventional method in which the biomass material is directly pyrolyzed, the method of the present invention, in which the pyrolysis treatment is performed after the acid washing pretreatment, not only increases the sugar content in the bio-oil, but also increases the yield of the bio-oil, wherein the sugar content in the bio-oil is increased from 2.8% to 42.13-51.52%, and the yield of the bio-oil is increased from 24.74 wt.% to 27.26-30.18 wt.%, overcomes the defects of low yield of the bio-oil, low sugar content, and the like in the conventional pyrolysis method, and has a very important meaning for increasing the resource utilization efficiency of the biomass material. Meanwhile, compared with the conventional pyrolysis (such as acid leaching, steam explosion or microwave treatment and acid combination) method, the method disclosed by the invention can effectively improve the yield and sugar content of the bio-oil, has the advantages of simple process, convenience in operation, mild conditions and the like, is suitable for preparing high-quality bio-oil on a large scale, and is beneficial to resource utilization of biomass materials and bio-oil.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (10)
1. A method for increasing the sugar content of biological oil, which is characterized by comprising the following steps:
s1, mixing the biomass material with an acid solution, stirring at a temperature of less than or equal to 70 ℃, standing, carrying out acid washing pretreatment on the biomass material, carrying out solid-liquid separation, washing, and drying to obtain an acid-washed biomass material;
s2, carrying out pyrolysis treatment on the acid-washed biomass material obtained in the step S1 to obtain the bio-oil with high sugar content.
2. The method of claim 1, wherein the stirring is performed at a temperature of 15 ℃ to 50 ℃ in step S1.
3. The method for increasing the sugar content in the bio-oil according to claim 2, wherein in the step S1, the stirring time is 2-5 h; the standing time is 0.5-1 h.
4. The method for increasing the sugar content in the bio-oil according to any one of claims 1 to 3, wherein in the step S1, the mass-to-volume ratio of the biomass material to the acid solution is 1 g: 10 mL; the acid solution is any one of hydrochloric acid, sulfuric acid, formic acid and acetic acid; the mass fraction of the acid solution is 1-7%.
5. The method for increasing the sugar content in the bio-oil according to claim 4, wherein the acid solution is 3 to 4% by mass in the step S1.
6. The method for increasing sugar content in bio-oil according to claim 4, wherein in step S1, the biomass material is rice hulls; the biomass material further comprises, prior to use: the biomass material is crushed to be less than or equal to 60 meshes.
7. The method for increasing the sugar content in the bio-oil according to any one of claims 1 to 3, wherein in the step S1, the solid-liquid separation is suction filtration of the acid washing pretreatment product; the washing is to wash the solid-liquid separation product by water until the pH value of the washing liquid is 7; the drying is carried out at the temperature of 85-105 ℃; the drying time is 24-48 h.
8. The method for increasing the sugar content in the bio-oil according to any one of claims 1 to 3, wherein in the step S2, the pyrolysis treatment is performed under the protection of nitrogen; the heating rate in the pyrolysis treatment process is 10 ℃/min; the temperature of the pyrolysis treatment is 550 ℃; the pyrolysis treatment time was 30 min.
9. The method for increasing the sugar content in the bio-oil according to any one of claims 1 to 3, wherein the pyrolysis treatment further comprises the following treatment in step S2: and (3) conveying a gas product generated in the pyrolysis treatment to an organic solvent by taking nitrogen or argon as a carrier gas for condensation, evaporating to remove the organic solvent in the obtained condensate, and collecting to obtain the biological oil with high sugar content.
10. The method of claim 9, wherein the organic solvent is acetone; the condensation is carried out under ice-water bath conditions; the temperature of the evaporation was 57 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113416565A (en) * | 2021-07-13 | 2021-09-21 | 华南农业大学 | Method for promoting pyrolysis saccharification by pretreating biomass raw material with simulated low cosolvent and application |
| US20230159831A1 (en) * | 2021-11-22 | 2023-05-25 | South China Agricultural University | Method for upgrading pyrolysis oil through seawater electrochemical pretreatment of biomass and use thereof |
| US11732196B2 (en) * | 2021-11-22 | 2023-08-22 | South China Agricultural University | Method for upgrading pyrolysis oil through seawater electrochemical pretreatment of biomass feedstock |
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