CN113416753A - Method for improving anaerobic digestion efficiency of organic waste by utilizing tire pyrolysis waste residues - Google Patents
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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Abstract
The invention belongs to the technical field of solid waste and water treatment processes, and discloses a method for improving anaerobic digestion efficiency of organic waste by utilizing tire pyrolysis waste residues. The method of the invention comprises the following steps: (1) waste tires are used as raw materials, crushed into colloidal particles, pyrolyzed and pyrolyzed, and N is used in the preparation process of pyrolytic carbon2As carrier gas, the relative air pressure is 0.007-0.012MPa, N2Heating the tube furnace to the target temperature at the speed of 7-13 ℃/min at the flow rate of not higher than 100mL/min, maintaining for 1.5-2.5 hours, then cooling to 350 ℃ at the speed of 7-13 ℃/min, cooling the product to room temperature, and drying for later use; (2) adding anaerobic sludge and vinegar residue into an anaerobic reactor, adding pyrolytic carbon, and anaerobically generating biogas at 32-37 ℃. The method uses pyrolytic carbon, which is solid waste produced under different pyrolysis conditions, as an additive material of an anaerobic reactor, and strengthens the fibrous organic waste represented by vinegar residueThe anaerobic treatment process improves the hydrolysis efficiency of the materials and the biochemical methane production potential.
Description
Technical Field
The invention relates to the technical field of solid waste and water treatment processes, in particular to a method for improving anaerobic digestion efficiency of organic waste by utilizing waste tire pyrolysis residues, and more particularly relates to a method for improving yield of volatile acid and methane in an anaerobic digestion process of easily degradable organic matters by utilizing pyrolytic carbon generated in a waste tire chemical pyrolysis process.
Background
The organic waste or high-concentration organic wastewater is suitable for being treated in an anaerobic digestion mode due to high organic matter content, so that the waste is recycled while organic matters are degraded, and volatile acid and methane are generated. However, in some materials, such as vinegar residue, straw, sludge, etc., since organic components thereof are wrapped by refractory substances, such as fibrous tissues, extracellular polymers, etc., microorganisms are difficult to contact and degrade, resulting in low treatment efficiency and low yield of volatile acids and methane in the anaerobic process.
In order to improve the anaerobic treatment efficiency, some mechanical or physicochemical means are often adopted to pretreat the materials, such as ultrasonic pretreatment, high-temperature and high-pressure pretreatment, acid-base pretreatment and the like. However, on the one hand, the pretreatment requires additional equipment investment or reaction structure construction; on the other hand, some of these methods have high energy consumption, and some of them require the use of a large amount of chemicals, which is expensive. Therefore, it is necessary to develop a method for improving anaerobic treatment efficiency, which is convenient and economical to operate.
At present, more than 4 hundred million waste tires are produced in China every year, the waste tires are subjected to resource treatment in a pyrolysis mode in the chemical field, pyrolysis oil and pyrolysis gas generated in the pyrolysis process are high-quality energy substitutes, and the generated residues, namely pyrolysis carbon, have low additional value. Although the pyrolytic carbon can be further processed into carbon black, the process chain length and the processing cost are high, and most of the pyrolytic carbon is not utilized and becomes new solid waste. The inventor analyzes the physicochemical property of the pyrolytic carbon and finds that the pyrolytic carbon has good specific surface area and good conductivity. Good conductive materials, such as activated carbon, carbon cloth, electrolytic cells and the like, can improve the metabolic activity of anaerobic methanogenesis, but the conductive materials adopted in the existing research have high manufacturing cost and larger size and occupy more effective space of the reactor.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provide a method for improving the anaerobic digestion efficiency of organic waste by using tire pyrolysis waste residues. According to the method, the solid waste-pyrolytic carbon generated by the waste tires under different pyrolysis conditions is researched, and the specific conductivity of the pyrolytic carbon is utilized to serve as an addition material of an anaerobic reactor, so that the anaerobic treatment process of fiber organic waste represented by vinegar residue is enhanced, and the hydrolysis efficiency and biochemical methane production potential of the material are improved.
In order to achieve the purpose of the invention, the method for improving the anaerobic digestion efficiency of organic waste by utilizing the tire pyrolysis waste residue comprises the following steps:
(1) the waste tires are taken as raw materials and crushed into colloidal particles, the colloidal particles are pyrolyzed at the temperature of 500-2Using a tube furnace as carrier gas, wherein the relative air pressure in the tube furnace is 0.007-0.012Mpa, N2Heating the tube furnace to the target temperature at the speed of 7-13 ℃/min at the flow rate of not higher than 100mL/min, maintaining for 1.5-2.5 hours, then cooling to 350 ℃ at the speed of 7-13 ℃/min, and placing the product into a dryer for later use after cooling to the room temperature;
(2) adding anaerobic sludge and vinegar residue into an anaerobic reactor, adding the pyrolytic carbon obtained in the step (1), and carrying out anaerobic biogas production at the temperature of 32-37 ℃.
Preferably, in some embodiments of the present invention, the relative gas pressure in the furnace in step (1) is 0.009-0.011MPa, N2The flow rate is not higher than 100mL/min, the heat pipe furnace is heated to the target temperature at the speed of 9-11 ℃/min and is maintained for 1.9-2.1 hours, and then the temperature is reduced to 290-310 ℃ at the speed of 9-11 ℃/min.
Preferably, in some embodiments of the present invention, the pyrolysis temperature in step (1) is 600-.
Further preferably, in some embodiments of the present invention, the pyrolysis temperature in step (1) is 900-.
Further, in some embodiments of the present invention, the mass ratio of the anaerobic sludge to the vinegar residue in the step (2) (calculated based on the mass of VS, VS is volatile solid, generally representing organic components in the solid) is 1-2: 1-3.
Preferably, in some embodiments of the present invention, the mass ratio of the anaerobic sludge to the vinegar residue in the step (2) (calculated based on the mass of VS, VS is volatile solid, generally representing organic components in the solid) is 1-2: 1-2.
Further, in some embodiments of the present invention, the mass ratio of the vinegar residue to the pyrolytic carbon in the step (2) is 4-8: 1.
further, in some embodiments of the present invention, the amount of the pyrolytic carbon added in the step (2) is greater than or equal to 10 g/L.
Preferably, in some embodiments of the present invention, the amount of the pyrolytic carbon added in the step (2) is greater than or equal to 20 g/L.
Further preferably, in some embodiments of the present invention, the amount of the pyrolytic carbon added in the step (2) is greater than or equal to 30 g/L.
The method does not need to further process and treat residual waste solids generated in the pyrolysis process of the waste tires in the chemical industry, and by optimizing and selecting the process parameters and utilizing the good conductivity of the pyrolytic carbon, the abundance of functional flora in an anaerobic system is effectively improved, the anaerobic treatment process of organic solid wastes, particularly organic wastes with high fiber content is promoted, the yield of volatile acid is improved, and the methane production potential of the organic solid wastes is further improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In the present invention, the pyrolysis process of the pyrolytic carbon can be a tire pyrolysis process which is conventional in the chemical industry, except for the specific examples. Furthermore, the description below of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily for the same embodiment or example. Further, the technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
Waste tires are used as raw materials and are crushed into colloidal particles of 2cm multiplied by 1cm, the colloidal particles are pyrolyzed at the temperature of 600-1000 ℃, in the process of preparing pyrolytic carbon,with N2Using a tube furnace as carrier gas, wherein the relative air pressure in the tube furnace is 0.01Mpa, N2Heating the tube furnace to the target temperature at the speed of 10 ℃/min at the flow rate of not more than 100mL/min, maintaining for 2 hours, then cooling to 300 ℃ at the speed of 10 ℃/min, and putting the product into a dryer after the product is cooled to the room temperature.
The pyrolysis carbon obtained by pyrolysis at 600-.
The specific surface area of the pyrolytic carbon is in the range of 600-1000 ℃, and the specific surface area is reduced along with the increase of the temperature, because the higher the temperature is, the micropores formed by the pyrolytic carbon at the low temperature collapse, so that the number of the micropores is reduced sharply, and the average pore diameter is increased (the higher the temperature is later, the more obvious the methane yield improvement effect is, the size of the specific surface area and the adsorption capacity of the pyrolytic carbon are not the main factors for determining the methane production effect). The conductivity increases with increasing temperature, because the content of organic impurities is reduced due to increasing pyrolysis temperature, so that the distance between conductive particles is shortened, and the conductivity is improved.
TABLE 1 comparison of the properties of the pyrolytic carbon of waste tires of the present invention and activated carbon
| Performance of | Pyrolytic carbon | Activated carbon |
| Conductivity (S/m) | (5.79-8.67)×104 | (3.03-6.89)×104 |
| Specific surface area(m2/g) | 25.8-39.1 | 800-1200 |
| Average pore diameter (nm) | 2.3-5.2 | 2.0-4.0 |
| Carbon element (%) | 92.8-96.7％ | - |
| Nitrogen element (%) | 0-3.7％ | - |
| Oxygen element (%) | 0.5-3.0％ | - |
| Sulfur element (%) | 0.4-2.2％ | - |
Example 2
Crushing waste tires as raw materials into colloidal particles of 2cm multiplied by 1cm, pyrolyzing the colloidal particles at 800 ℃, and using N in the preparation process of pyrolytic carbon2Using a tube furnace as carrier gas, wherein the relative air pressure in the tube furnace is 0.01Mpa, N2Heating the tube furnace to the target temperature at the speed of 10 ℃/min at the flow rate of not more than 100mL/min, maintaining for 2 hours, then cooling to 300 ℃ at the speed of 10 ℃/min, and putting the product into a dryer for later use after the product is cooled to the room temperature;
respectively mixing anaerobic sludge and vinegar residue 1:1 and 1: two inoculum ratios (VS is a volatile solid, based on VS mass, usuallyRepresenting organic components in the solid) to an anaerobic reactor with a total volume of 0.6L (an effective material volume of 0.4L), adding anaerobic sludge and vinegar residue, adding 20g/L (8 g) of the obtained pyrolytic carbon, and anaerobically generating biogas at 35 ℃. Compared with a control group reactor with the same inoculation ratio but without adding the pyrolytic carbon, the methane yield is respectively from 182mLCH4gVS and 178.5mLCH4lifting/gVS to 285.8mLCH4PergVS and 287.4mLCH4and/gVS, and the lifting rates reach 57% and 61% respectively.
Example 3
Crushing waste tires as raw materials into colloidal particles of 2cm multiplied by 1cm, pyrolyzing the colloidal particles at 800 ℃, and using N in the preparation process of pyrolytic carbon2Using a tube furnace as carrier gas, wherein the relative air pressure in the tube furnace is 0.01Mpa, N2Heating the tube furnace to the target temperature at the speed of 10 ℃/min at the flow rate of not more than 100mL/min, maintaining for 2 hours, then cooling to 300 ℃ at the speed of 10 ℃/min, and putting the product into a dryer for later use after the product is cooled to the room temperature.
Mixing anaerobic sludge and vinegar residue 1: 3 (calculated based on VS mass) anaerobic sludge and vinegar residue were added to an anaerobic reactor having a material volume of 0.4L, and 20g/L (i.e., 8g) of the above-obtained pyrolytic carbon was added, and anaerobic biogas production was carried out at 35 ℃. Because the addition amount of the vinegar residue is too large and the organic load is too high, the control group reactor has a severe acidification phenomenon, and the yield of the methane is only 43.1mLCH4The reaction group added with 8g of pyrolytic carbon has the methane yield of 225.9mLCH in the same reaction period along with the elimination of acidification phenomenon although the reaction also has the phenomenon of gas production retardation4and/gVS. This example shows that the pyrolytic carbon not only improves the biochemical methanogenesis potential of the material, but also alleviates the "over-acidification" phenomenon that may occur during high load anaerobic processes.
Example 4
The waste tires are taken as raw materials and crushed into colloidal particles of 2cm multiplied by 1cm, the colloidal particles are pyrolyzed at the temperature of 600-1000 ℃, and N is used in the preparation process of the pyrolytic carbon2Using a tube furnace as carrier gas, wherein the relative air pressure in the tube furnace is 0.01Mpa, N2The flow rate is not higher than 100mL/min, and the temperature is increased at the rate of 10 ℃/minHeating the tube furnace to the target temperature and maintaining for 2 hours, then cooling to 300 ℃ at the speed of 10 ℃/min, and putting the product into a dryer for later use after cooling to the room temperature.
Mixing anaerobic sludge and vinegar residue 1:1 (calculated based on VS mass), adding anaerobic sludge and vinegar residue into different anaerobic reactors (the effective volumes of materials are all 0.4L), wherein the corresponding organic load is 15gVS/L, and respectively adding 10g/L, 20g/L (namely 8g) and 30g/L of the pyrolytic carbon obtained by 600-plus-1000 ℃ pyrolysis, compared with a control reactor without the pyrolytic carbon, the efficiency of improving the methane yield is shown in Table 2.
Table 2 efficiency of increasing yield of methane from anaerobic digestion of vinegar residue by pyrolytic carbon obtained from different parameters
As can be seen from Table 2, the pyrolysis temperature and the addition amount play a decisive role in promoting the anaerobic methanogenesis effect by the pyrolytic carbon. The methane yield increasing effect of the organic matters is increased along with the increase of the adding amount and the pyrolysis temperature.
Example 5
In an anaerobic reactor with an effective material volume of 0.4L and an anaerobic sludge-vinegar residue inoculation ratio of 1:1 (calculated based on VS mass), a methane production process inhibitor is added to avoid the consumption of volatile acid, pyrolytic carbon generated at different pyrolysis temperatures is added into three reactors respectively, and the influence of the pyrolytic carbon on the yield of the volatile acid in the acid production stage of anaerobic hydrolysis is researched. The results show that after the reactor is added with 20g/L (namely 8g) of pyrolytic carbon at 600 ℃, 800 ℃ and 1000 ℃ and the reaction is carried out for 7 days, the yield of the volatile acid in each reactor is 2600mg/L, 2941mg/L and 3330mg/L respectively, and the yield is improved by 20.9%, 36.8% and 54.9% respectively compared with the reactor (2150mg/L) of a control group without the pyrolytic carbon.
The yield of acetic acid in the three reactors added with pyrolytic carbon is 1582mg/L, 1934mg/L and 2247mg/L respectively, and is increased by 16.0%, 41.8% and 64.7% respectively compared with the yield of acetic acid in a reactor (1364mg/L) in a control group without pyrolytic carbon.
Comparative example 1
Compared with the effect of adding waste tires to prepare pyrolytic carbon and active carbon on the anaerobic methane production efficiency of the vinegar residue, 20g/L (8 g) of pyrolytic carbon anaerobic reactor with the pyrolysis temperature of 1000 ℃ and the methane yield of 258 +/-23 mLCH is added into an anaerobic reactor with the inoculation ratio of anaerobic sludge to the vinegar residue of 2:1 and the effective material volume of 0.4L under the lower load condition that the corresponding organic load of the vinegar residue is 7.5gVS/L4/gVS, while the methane yield of the anaerobic reactor fed with commercial activated carbon with the same mass is 262 +/-15 mLCH4(iv)/gVS, all slightly higher than the methane yield of the control reactor 241 + -18 mLCH4and/gVS. This indicates that the pyrolysis carbon has a similar methane-generating promoting effect to that of activated carbon under low load conditions.
Comparative example 2
In an anaerobic reactor (effective volume 0.4L) with anaerobic sludge and vinegar residue inoculation ratios of 1:1 and 1:2, the methane yield of a reactor which is added with 20g/L (8 g) of pyrolytic carbon with the pyrolysis temperature of 1000 ℃ is 265mLCH corresponding to the organic load of the vinegar residue of 15gVS/L and 25gVS/L4/gVS and 282mLCH4(gVS), the methane yield is 238mLCH respectively compared with an anaerobic reactor added with the same amount of commercial activated carbon4/gVS and 261mLCH4The promotion effect of the pyrolytic carbon on the methane production of the vinegar residue is obviously better than that of the activated carbon. The reason is that the conductivity of the pyrolytic carbon is stronger than that of the active carbon, so that the inter-species electron transfer efficiency of microorganisms in the metabolic process of methanogenesis is accelerated.
Comparative example 3
The inoculation ratio of anaerobic sludge to vinegar residue is 1: 3 (effective material volume 0.4L), the control reactor showed severe acidification as in example 3, and the methane production process could not be performed normally. The final methane yield of the reactor, which is added with 20g/L (8 g) of pyrolytic carbon with the pyrolysis temperature of 1000 ℃, is 230.1mLCH4gVS, the time from the beginning of acidification to the recovery of normal gas production is 8 days, and the addition of the same amount of commercial activated carbon can also make the reactor recover normal gas production from the acidification state, the recovery period is 12 days, and the final methane yield is 211.6mLCH4and/gVS. Therefore, the effect of the pyrolytic carbon produced by the method from the perspective of eliminating acidification phenomenon is also due to commercial productsActivated carbon.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.
Claims (10)
1. A method for improving the anaerobic digestion efficiency of organic waste by using tire pyrolysis waste residue, which is characterized by comprising the following steps:
(1) the waste tires are taken as raw materials and crushed into colloidal particles, the colloidal particles are pyrolyzed at the temperature of 500-2Using a tube furnace as carrier gas, wherein the relative air pressure in the tube furnace is 0.007-0.012Mpa, N2Heating the tube furnace to the target temperature at the speed of 7-13 ℃/min at the flow rate of not higher than 100mL/min, maintaining for 1.5-2.5 hours, then cooling to 350 ℃ at the speed of 7-13 ℃/min, and placing the product into a dryer for later use after cooling to the room temperature;
(2) adding anaerobic sludge and vinegar residue into an anaerobic reactor, adding the pyrolytic carbon obtained in the step (1), and carrying out anaerobic biogas production at the temperature of 32-37 ℃.
2. The method for improving the anaerobic digestion efficiency of organic wastes using the tire pyrolysis residue as claimed in claim 1, wherein the relative air pressure in the furnace in the step (1) is 0.009-0.011MPa, N2The flow rate is not higher than 100mL/min, the heat pipe furnace is heated to the target temperature at the speed of 9-11 ℃/min and is maintained for 1.9-2.1 hours, and then the temperature is reduced to 290-310 ℃ at the speed of 9-11 ℃/min.
3. The method for improving the anaerobic digestion efficiency of organic wastes by utilizing the tire pyrolysis waste residues as claimed in claim 1, wherein the pyrolysis temperature in the step (1) is 600-1000 ℃.
4. The method for improving the anaerobic digestion efficiency of organic wastes by utilizing the tire pyrolysis waste residues as claimed in claim 1, wherein the pyrolysis temperature in the step (1) is 900-1100 ℃.
5. The method for improving the anaerobic digestion efficiency of organic wastes by using the tire pyrolytic waste residues according to claim 1, wherein the mass ratio of the anaerobic sludge to the vinegar residues in the step (2) is 1-2: 1-3.
6. The method for improving the anaerobic digestion efficiency of organic wastes by using the tire pyrolytic waste residues according to claim 1, wherein the mass ratio of the anaerobic sludge to the vinegar residues in the step (2) is 1-2: 1-2.
7. The method for improving the anaerobic digestion efficiency of organic wastes by using the tire pyrolytic waste residues according to claim 1, wherein the mass ratio of the vinegar residue to the pyrolytic carbon in the step (2) is 4-8: 1.
8. the method for improving the anaerobic digestion efficiency of organic wastes by using the tire pyrolytic waste residue according to claim 1, wherein the addition amount of the pyrolytic carbon in the step (2) is greater than or equal to 10 g/L.
9. The method for improving the anaerobic digestion efficiency of organic wastes by using the tire pyrolytic waste residue according to claim 1, wherein the addition amount of the pyrolytic carbon in the step (2) is greater than or equal to 20 g/L.
10. The method for improving the anaerobic digestion efficiency of organic wastes by using the tire pyrolytic waste residue according to claim 1, wherein the addition amount of the pyrolytic carbon in the step (2) is greater than or equal to 30 g/L.
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