CN115029148A - Method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic - Google Patents
Method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic Download PDFInfo
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- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
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- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
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Abstract
The invention discloses a method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic, which specifically comprises the following steps: mixing the crushed biomass with MgCl 2 After being uniformly dipped and mixed, the raw materials are uniformly and mechanically mixed with polyolefin plastics to obtain pyrolysis raw materials; the pyrolysis raw material and the molecular sieve catalyst are separately placed in a two-section fixed bed reactor, and the fast pyrolysis reaction is carried out in the nitrogen atmosphere; cooling volatile matters generated by fast pyrolysis by adopting an ice-water mixture, and collecting liquid products to obtain high-quality bio-oil; further heating the pyrolysis raw material to carry out slow pyrolysis to improve the modification degree of the biocharThen collecting the solid product, washing and drying to obtain the mesoporous biochar. The method has the advantages of low cost, convenient operation and capability of stably and efficiently co-producing high-quality bio-oil and mesoporous biochar. The invention is beneficial to realizing high-value utilization of biomass waste.
Description
Technical Field
The invention belongs to the field of biomass utilization, and particularly relates to a method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic.
Background
As the only renewable energy source containing carbon, the biomass has the advantages of huge reserves, wide distribution, stable sources, low price, easy obtainment and the like. The pyrolysis technology is considered to be one of the most promising biomass utilization technologies due to the characteristics of full-component conversion, high utilization efficiency, strong raw material adaptability, simple device and the like. Pyrolysis gas obtained by biomass pyrolysis can supply heat for biomass pyrolysis, so that energy self-sufficiency is realized; the bio-oil is expected to be used as a substitute fuel of gasoline and diesel, and organic components in the bio-oil can be used for preparing high value-added chemicals after separation and purification; the biochar can be used as a high-grade solid fuel and further processed into an adsorbent, an electrode material and the like. However, the bio-oil obtained by conventional pyrolysis of biomass has the disadvantages of high oxygen content, strong acidity, poor stability and the like, and the porosity of the biochar is low, which seriously hinders the popularization and application of the bio-oil.
Compared with the conventional biomass pyrolysis, the oxygen-enriched biomass and the hydrogen-enriched polyolefin plastic are subjected to co-catalytic pyrolysis under the action of the molecular sieve, so that the biomass pyrolysis volatile component is promoted to be deoxidized through the interaction between the biomass pyrolysis volatile component and the polyolefin plastic pyrolysis volatile component, and the quality of the bio-oil is further improved.
Current co-catalytic pyrolysis technologies typically use zeolitic molecular sieves (e.g., ZSM-5 molecular sieves) as catalysts. Because the biomass pyrolysis volatile component is relatively complex, and the plastic polyolefin plastic pyrolysis volatile component contains a large amount of long-chain hydrocarbon substances, the interaction of the biomass pyrolysis volatile component and the polyolefin plastic pyrolysis volatile component on a molecular sieve interface is relatively weak, and the quality of the bio-oil is still to be further improved. On the other hand, the current co-catalytic pyrolysis technology has less attention to the biochar, and the yield of the biochar in the co-catalytic pyrolysis product of the biomass and the polyolefin plastic is 15% -35%, so that the biochar is low in quality and difficult to apply, and the co-catalytic pyrolysis technology is poor in economy.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastics, which improves the added value of products and has the advantages of low cost, simple process and continuous and efficient preparation of biomass-based products.
In order to achieve the above object, according to one aspect of the present invention, a method for co-producing high quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic is provided, which is characterized by comprising the following steps:
s1, crushing the biomass into particles of 60-100 meshes, and mixing the biomass and MgCl according to a mass ratio of 4: 1-19: 1 2 Uniformly mixing by an impregnation mode, evaporating to remove water and drying to obtain MgCl 2 A modified biomass sample;
s2, crushing polyolefin plastic into particles of 60-100 meshes, drying, and mixing the polyolefin plastic and MgCl according to a mass ratio of 1: 5-1: 1 2 Uniformly mixing the modified biomass samples in a mechanical stirring manner to obtain a pyrolysis raw material;
s3, respectively placing a pyrolysis raw material and a ZSM-5 molecular sieve catalyst in an upper section and a lower section of a two-section fixed bed reactor, performing rapid pyrolysis reaction in a nitrogen atmosphere, and reforming volatile components generated by the pyrolysis raw material reaction through a 600 ℃ molecular sieve bed layer, wherein the temperature of the upper section of the fixed bed reactor is 500-600 ℃, the reaction time is 10min, and the mass ratio of the pyrolysis raw material to the molecular sieve is 1: 8-1: 4;
s4, cooling the volatile components reformed in the step S3 by adopting an ice-water mixture, and collecting liquid products to obtain high-quality bio-oil products;
s5, slowly raising the temperature of the upper section of the reactor in the step S3 to 650-800 ℃ at a speed of 5 ℃/min, preserving the temperature for 30min to strengthen the modification process of the biochar, pickling the solid product obtained after the reaction is finished, filtering and washing the solid product with excessive deionized water until the filtrate is neutral, and drying the filtrate to obtain the mesoporous biochar.
Further, the biomass in the step S1 is one or more of cotton stalk, wheat straw, chestnut shell and bamboo dust.
Further, the temperature for evaporating the water in the step S1 is 35-65 ℃, the drying temperature is 35-65 ℃, and the drying time is 12-24 hours.
Further, the polyolefin plastic in the step S2 is one or more of low density polyethylene, high density polyethylene, and polypropylene.
Further, the drying temperature in the step S2 is 35-65 ℃, and the drying time is 12-24 h.
Further, the main components of the high-quality bio-oil in step S4 are benzene, toluene, and p-toluene.
Further, the acid washing in the step S5 is performed by using a hydrochloric acid solution, the concentration of the hydrochloric acid solution is 0.5-1 mol/L, the drying temperature is 105 ℃, and the drying time is 12-24 hours.
Generally, compared with the prior art, the technical scheme conceived by the invention mainly has the following technical advantages:
(1) the method of the invention skillfully utilizes MgCl 2 The biomass pyrolysis volatile matter and the polyolefin plastic pyrolysis volatile matter are respectively reformed by MgO obtained by conversion in the pyrolysis process, the interaction of the biomass pyrolysis volatile matter and the polyolefin plastic pyrolysis volatile matter on a ZSM-5 molecular sieve interface is enhanced by simplifying the composition of the biomass pyrolysis volatile matter and promoting the generation of short-chain hydrocarbon, the quality of the bio-oil is improved, other catalysts do not need to be additionally introduced to simultaneously realize the regulation and control of the biomass pyrolysis volatile matter and the polyolefin plastic pyrolysis volatile matter, and the cost of the catalysts is reduced.
(2) The method of the invention obtains high-quality bio-oil and simultaneously passes through MgCl 2 The catalytic action and the MgO template action ensure that the pore structure of the biochar is improved to a great extent, and the biochar realizes the purpose of improving the pore structure in the same reactorThe co-production of the high-quality bio-oil and the mesoporous bio-carbon reduces the complexity of the operation.
(3) The method combines the low-temperature stage fast pyrolysis and the high-temperature stage slow pyrolysis, optimizes reaction parameters, realizes the consideration of the quality improvement of the bio-oil and the quality improvement of the mesoporous biochar, and greatly improves the economy of the co-catalytic pyrolysis technology.
(4) The catalyst and the pyrolysis raw material are separately placed, so that the coke product and the catalyst are convenient to recycle, the problem of resource waste in the traditional catalytic pyrolysis process is solved, the pyrolysis gas obtained in the method can supply heat for biomass pyrolysis, the self-sufficiency of energy in the pyrolysis process is realized, and the utilization efficiency of biomass energy is improved.
Drawings
Fig. 1 is a flowchart of a method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, the method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic provided by the embodiment of the invention specifically includes the following steps:
(1) crushing biomass into particles of 60-100 meshes, and mixing the biomass and MgCl according to a mass ratio of 4: 1-19: 1 2 Uniformly mixing by dipping, evaporating water and drying to obtain MgCl 2 A modified biomass sample;
(2) crushing polyolefin plastics into particles of 60-100 meshes, drying, and mixing the polyolefin plastics and MgCl according to a mass ratio of 1: 5-1: 1 2 Uniformly mixing the modified biomass samples in a mechanical stirring manner to obtain a pyrolysis raw material;
(3) respectively placing a pyrolysis raw material and a ZSM-5 molecular sieve catalyst in an upper section and a lower section of a two-section fixed bed reactor, performing fast pyrolysis reaction in a nitrogen atmosphere, and reforming volatile components generated by the pyrolysis raw material reaction through a 600 ℃ molecular sieve bed layer, wherein the temperature of the upper section of the fixed bed reactor is 500-600 ℃, the reaction time is 10min, and the mass ratio of the pyrolysis raw material to the molecular sieve is 1: 8-1: 4;
(4) cooling the volatile matter reformed in the step (3) by adopting an ice water mixture, and collecting a liquid product to obtain a high-quality bio-oil product;
(5) and (4) raising the temperature of the upper section of the reactor in the step (3) to 650-800 ℃ at a low speed of 5 ℃/min, preserving the temperature for 30min to strengthen the modification process of the biochar, pickling the solid product obtained after the reaction is finished, filtering and washing the solid product with excessive deionized water until the filtrate is neutral, and drying the filtrate to obtain the mesoporous biochar.
Wherein the biomass in the step (1) is one or more of cotton stalks, wheat straws, chestnut shells and bamboo scraps.
The temperature for evaporating water in the step (1) is 35-65 ℃, the drying temperature is 35-65 ℃, and the drying time is 12-24 h.
The polyolefin plastic in the step (2) is one or more of low-density polyethylene, high-density polyethylene and polypropylene.
The drying temperature in the step (2) is 35-65 ℃, and the drying time is 12-24 h.
The main components of the high-quality bio-oil in the step (4) are benzene, toluene and p-toluene.
And (5) acid washing is carried out by adopting a hydrochloric acid solution, wherein the concentration of the hydrochloric acid solution is 0.5-1 mol/L, the drying temperature is 105 ℃, and the drying time is 12-24 hours.
The principle of the invention concept is as follows: (1) the biological oil quality is improved: in the low temperature pyrolysis stage, MgCl 2 The catalytic action of (A) simplifies the pyrolysis volatile components of the biomass, reduces unstable phenolic substances and high-oxygen-content carbohydrate substances, and part of MgCl is generated when the temperature is increased 2 Converting into MgO, depolymerizing polyolefin plastics, and converting long-chain hydrocarbon into short-chain hydrocarbon under catalytic action of MgOA hydrocarbon. The reforming process enhances the interaction of the biomass pyrolysis volatile component and the polyolefin plastic pyrolysis volatile component on the molecular sieve interface, and further improves the quality of the bio-oil. (2) The quality of the biochar is improved: in the low temperature pyrolysis stage, MgCl 2 The pores of the biochar are promoted by catalytic dehydration and the like, and MgCl is formed after the temperature is increased 2 Converted into MgO, and the template function of the MgO can also improve the pores of the biochar. (3) The joint production of the bio-oil and the bio-carbon comprises the following steps: in order to shorten the time interval between the pyrolysis volatile components of the biomass and the pyrolysis volatile components of the polyolefin plastics as much as possible, so that the pyrolysis volatile components of the biomass and the pyrolysis volatile components of the polyolefin plastics pass through the molecular sieve bed layer as much as possible, and the interaction between the two volatile components is strengthened, a fast heating rate and a relatively low temperature need to be adopted. And a slower heating rate and a higher temperature are needed to improve the modification degree of the biochar. Therefore, the method adopts the modes of low-temperature stage fast pyrolysis and high-temperature stage slow pyrolysis to treat the pyrolysis raw materials, and realizes the co-production of high-quality bio-oil and mesoporous biochar.
To illustrate the process of the present invention in more detail, the following preferred examples are given to illustrate the practice of the present invention.
Example 1
The embodiment illustrates a method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastic, which specifically comprises the following steps:
(1) crushing cotton stalks into particles of 60-100 meshes, and mixing the cotton stalks with MgCl according to a mass ratio of 7:1 2 Uniformly mixing by dipping, evaporating to remove water at 35 ℃, and drying in an oven at 55 ℃ for 24 hours to obtain MgCl 2 A modified biomass sample;
(2) crushing low-density polyethylene plastics into particles of 60-100 meshes, then placing the particles in a 55 ℃ oven for drying for 24 hours, and mixing the polyolefin plastics and MgCl according to the mass ratio of 1:1 2 Uniformly mixing the modified biomass samples in a mechanical stirring manner to obtain a pyrolysis raw material;
(3) the catalytic cracking is carried out by using a two-section fixed bed reactor, the pyrolysis raw material and the ZSM-5 molecular sieve catalyst are respectively placed at the top end of the upper section of the reactor and in a hanging basket in the middle of the lower section of the reactor before the pyrolysis process begins, and then the upper section and the lower section of the reactor are respectively heated to 550 ℃ and 600 ℃. Then, the hanging basket filled with the pyrolysis raw material is quickly placed in the middle of the upper section of the reactor, and the volatile component generated by depolymerization of the pyrolysis raw material under the action of nitrogen is catalytically reformed through a ZSM-5 molecular sieve catalyst bed layer. Wherein the mass ratio of the pyrolysis raw material to the ZSM-5 molecular sieve catalyst is 1:4, and the reaction time is 10 min;
(4) cooling the reformed volatile components in the step (3) by adopting an ice-water mixture, and collecting liquid products to obtain high-quality bio-oil products;
(5) and (4) slowly raising the temperature of the upper section of the reactor in the step (3) to 700 ℃ at the speed of 5 ℃/min, and preserving the temperature for 30min to strengthen the modification process of the biochar. And (3) carrying out acid washing on the solid product obtained after the reaction is finished by using 0.5mol/L hydrochloric acid solution, filtering and washing by using excessive deionized water until the filtrate is neutral, and then drying the washed solid product in a drying oven at 105 ℃ for 24 hours to obtain the mesoporous biochar.
Comparative example 1
The comparative example illustrates a method for preparing high-quality bio-oil by co-catalytic pyrolysis of traditional biomass and polyolefin plastic, which specifically comprises the following steps:
(1) crushing a cotton stalk into particles of 60-100 meshes, and then drying in a drying oven at 55 ℃ for 24 hours to obtain a biomass sample;
(2) crushing low-density polyethylene plastics into particles of 60-100 meshes, then drying in an oven at 55 ℃ for 24 hours, and uniformly mixing the polyolefin plastics and a biomass sample in a mechanical stirring manner according to a mass ratio of 1:1 to obtain a pyrolysis raw material;
(3) the catalytic cracking is carried out by using a two-section fixed bed reactor, the pyrolysis raw material and the ZSM-5 molecular sieve catalyst are respectively placed at the top end of the upper section of the reactor and in a hanging basket in the middle of the lower section of the reactor before the pyrolysis process begins, and then the upper section and the lower section of the reactor are both heated to 600 ℃. Then, the hanging basket filled with the pyrolysis raw material is quickly placed in the middle of the upper section of the reactor, and the volatile component generated by depolymerization of the pyrolysis raw material under the action of nitrogen is catalytically reformed through a ZSM-5 molecular sieve catalyst bed layer. Wherein the mass ratio of the pyrolysis raw material to the ZSM-5 molecular sieve catalyst is 1:4, and the reaction time is 10 min;
(4) and (4) cooling the volatile components reformed in the step (3) by using an ice-water mixture, collecting liquid products to obtain a bio-oil product, and collecting solid products to obtain a biochar product.
Through gas chromatography-mass spectrometry combined test, the selectivity of monocyclic aromatic hydrocarbon (benzene, toluene and p-toluene) in the high-quality bio-oil in example 1 is 80%, and the yield (peak area) is 1.35E + 9; the selectivity to monocyclic aromatics (benzene, toluene, p-toluene) in the bio-oil of comparative example 1 was 72%, and the yield (peak area) was 1.20E + 9. In addition, the pore characteristic characterization test finds that the mesoporous biochar obtained in the example 1 has a developed pore structure, and the specific surface area reaches 475m 2 The proportion of mesopores is 85 percent; the specific surface area of the biochar in comparative example 1 was 102m 2 (ii)/g, and the proportion of micropores is 92%. In conclusion, the method can obviously improve the yield and selectivity of monocyclic aromatic hydrocarbons (benzene, toluene and p-toluene) in the bio-oil, can obviously improve the specific surface area and the mesoporous content of the biochar, and can be used for obtaining the mesoporous biochar.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A method for co-producing high-quality bio-oil and mesoporous biochar by catalytic pyrolysis of biomass and polyolefin plastics is characterized by comprising the following steps:
s1, crushing the biomass into particles of 60-100 meshes, and mixing the biomass and MgCl according to a mass ratio of 4: 1-19: 1 2 Uniformly mixing by dipping, evaporating water and drying to obtain MgCl 2 A modified biomass sample;
s2, crushing polyolefin plastic into particles of 60-100 meshes, drying, and mixing the polyolefin plastic and MgCl according to a mass ratio of 1: 5-1: 1 2 Modification ofUniformly mixing the biomass samples in a mechanical stirring manner to obtain a pyrolysis raw material;
s3, respectively placing a pyrolysis raw material and a ZSM-5 molecular sieve catalyst in an upper section and a lower section of a two-section fixed bed reactor, performing rapid pyrolysis reaction in a nitrogen atmosphere, and reforming volatile components generated by the pyrolysis raw material reaction through a 600 ℃ molecular sieve bed layer, wherein the temperature of the upper section of the fixed bed reactor is 500-600 ℃, the reaction time is 10min, and the mass ratio of the pyrolysis raw material to the molecular sieve is 1: 8-1: 4;
s4, cooling the volatile components reformed in the step S3 by adopting an ice-water mixture, and collecting liquid products to obtain high-quality bio-oil products;
s5, slowly raising the temperature of the upper section of the reactor in the step S3 to 650-800 ℃ at a speed of 5 ℃/min, preserving the temperature for 30min to strengthen the modification process of the biochar, pickling the solid product obtained after the reaction is finished, filtering and washing the solid product with excessive deionized water until the filtrate is neutral, and drying the filtrate to obtain the mesoporous biochar.
2. The method for co-producing high-quality bio-oil and mesoporous biochar through catalytic pyrolysis of biomass and polyolefin plastics according to claim 1, wherein the biomass in the step S1 is one or more of cotton stalks, wheat straws, chestnut shells and bamboo shavings.
3. The method for co-production of high-quality bio-oil and mesoporous biochar through catalytic pyrolysis of biomass and polyolefin plastic according to claim 1, wherein the temperature of water evaporated to dryness in step S1 is 35-65 ℃, the drying temperature is 35-65 ℃, and the drying time is 12-24 hours.
4. The method for co-producing high-quality bio-oil and mesoporous biochar through catalytic pyrolysis of biomass and polyolefin plastics according to claim 1, wherein the polyolefin plastics in the step S2 are one or more of low-density polyethylene, high-density polyethylene and polypropylene.
5. The method for co-producing the high-quality bio-oil and the mesoporous bio-carbon through catalytic pyrolysis of the biomass and the polyolefin plastic according to claim 1, wherein the drying temperature in the step S2 is 35-65 ℃, and the drying time is 12-24 hours.
6. The method for co-producing high-quality bio-oil and mesoporous biochar through catalytic pyrolysis of biomass and polyolefin plastics according to claim 1, wherein the main components of the high-quality bio-oil in the step S4 are benzene, toluene and p-toluene.
7. The method for co-production of high-quality bio-oil and mesoporous biochar through catalytic pyrolysis of biomass and polyolefin plastic according to claim 1, wherein acid washing in the step S5 is performed by using a hydrochloric acid solution, the concentration of the hydrochloric acid solution is 0.5-1 mol/L, the drying temperature is 105 ℃, and the drying time is 12-24 hours.
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