Biological environment-friendly asphalt and preparation method thereof

Abstract

The invention relates to the field of high polymer materials, in particular to biological environment-friendly asphalt and a preparation method thereof. The method comprises the following steps: (1) preparing solid carbon particles, biomass heavy oil and biomass light oil, and recovering nitrogen; (2) vaporizing the biomass heavy oil and introducing the vaporized biomass heavy oil into the plastic base material to prepare a prefabricated doping material; and (3) uniformly mixing the matrix asphalt, the recycled rubber granules, the auxiliary agent, the filler and the prefabricated doping material according to a ratio and process conditions to obtain the biological environment-friendly asphalt. According to the scheme, the biological type environment-friendly asphalt fully combines the properties of plastic, rubber and asphalt, and the prepared biological type environment-friendly asphalt is suitable for most use environments in needle penetration, ductility and softening temperature; meanwhile, biomass heavy oil and biomass light oil are fully utilized in the process, waste heat in nitrogen is recycled, and energy is saved.

Description

Technical Field

[0001] The present invention relates to the field of polymer materials, and particularly to a biological environmental protection type asphalt and a preparation method thereof. Background Art

[0002] Asphalt is an important petrochemical industrial raw material, mainly used in fields such as road paving, waterproof building, and rubber industry. With the continuous progress of road construction and maintenance projects in China, the market demand for asphalt has been continuously increasing. However, petroleum resources, which are the main source of asphalt, are limited and non-renewable, which has led to the risk of imbalance in the supply and demand relationship of traditional petroleum asphalt. Biomass resources are abundant and cheap, and it is also technically feasible to replace or modify petroleum asphalt with biomass heavy oil. However, processes such as pyrolysis for preparing biomass heavy oil consume a large amount of energy. At the same time, biomass heavy oil improves the fluidity of asphalt, increases the penetration, and reduces the softening temperature.

[0003] CN 114752108 B discloses a method for degrading waste tire rubber into asphalt-like material. The method for degrading waste tire rubber into asphalt-like material includes the following steps: S1. Under an inert gas atmosphere, grind the waste tire rubber into powder, and successively add an organic solvent, an alkali, and a metal element to the powder, and degrade at 140 - 300 °C for 8 - 24 hours to obtain a degradation product mixture; S2. Add water to the degradation product mixture for stratification, filter, and recover the organic layer under reduced pressure to obtain asphalt-like material; the mass ratio of the powder, the organic solvent, the alkali, and the metal element is 1:(30 - 100):(0.1 - 0.5):(0.1 - 0.5). This invention has the advantage of high efficiency in recovering natural rubber and synthetic rubber through the addition of an organic solvent. The addition of the alkali enables the organic solvent to blend with rubber hydrocarbons, so that the properties of the asphalt-like viscous material obtained by the degradation reaction are close to those of commercially available asphalt.

[0004] CN 111253761 B proposes an environment-friendly biomass asphalt rejuvenator and a preparation method thereof. Among them, the environment-friendly biomass asphalt rejuvenator is composed of plant asphalt, naphthenic rubber oil, epoxy soybean oil, mixed fatty acid glyceride, antioxidant 770, and anti-stripping agent; the mass ratio of plant asphalt, naphthenic rubber oil, epoxy soybean oil, mixed fatty acid glyceride, antioxidant 770, and anti-stripping agent is 70.11:16.14:5.25:4.18:2.14:2.18. The beneficial technical effect of the present invention is: an environment-friendly biomass asphalt rejuvenator and a preparation method thereof are proposed. This environment-friendly biomass asphalt rejuvenator can not only effectively rejuvenate aged asphalt, but also has a low cost and less harmful substance content.

[0005] The above technologies do not mention how to reduce energy consumption and how to introduce biomass heavy oil while still ensuring that the fluidity, penetration, and softening temperature of asphalt are suitable for most application environments. Summary of the Invention

[0006] To solve the above problems, the present invention provides a bio-based environmentally friendly asphalt and its preparation method. The prepared bio-based environmentally friendly asphalt has good fluidity, and at the same time, its penetration, ductility, and softening temperature basically meet all application environments. It also has the characteristics of wide sources of production raw materials, low production energy consumption, and environmental protection.

[0007] To achieve the above object, the technical solution of the present invention is as follows:

[0008] A preparation method of a bio-based environmentally friendly asphalt, comprising the following steps:

[0009] Step (1): Dry the biomass raw material at 120°C to 150°C in a nitrogen environment until the water content is lower than 0.5%. After cleaning with low-temperature nitrogen, quickly heat it up to 450°C to 550°C, react for 3 minutes to 5 minutes, and then introduce continuous high-temperature nitrogen to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil and light oil-containing nitrogen. Pass the light oil-containing nitrogen into the second liquefaction tank for liquefaction to obtain biomass light oil and recycled nitrogen;

[0010] Step (2): By weight, heat and vaporize 5 parts to 10 parts of the biomass heavy oil obtained in step (1) and introduce it into 10 parts to 20 parts of the plastic substrate, and continuously stir until the plastic substrate is completely melted. Then add 1 part to 3 parts of the mixture of the biomass light oil and solid carbon particles obtained in step (1), and continue to stir to obtain a prefabricated doping material;

[0011] Step (3): By weight, heat 10 parts to 20 parts of the matrix asphalt, 5 parts to 8 parts of the recycled rubber particle material, 0.1 part to 2 parts of the additive, and 1 part to 3 parts of the filler to 130°C to 180°C under the condition of recycled nitrogen. Then add 3 parts to 5 parts of the prefabricated doping material, and mix evenly to obtain the bio-based environmentally friendly asphalt.

[0012] The purpose of this solution is to prepare a bio-based environmentally friendly asphalt. This solution has the following characteristics:

[0013] 1. Biomass raw materials are selected to prepare biomass heavy oil, solid carbon particles and biomass light oil. The biomass raw materials selected in this scheme are organic solid wastes, including crop straws, garden trimming plant branches and leaves, animal feces, kitchen waste, wood processing scraps, etc. The biomass heavy oil contains more asphalt light components and can be well integrated with matrix asphalt; the biomass light oil is similar to a plasticizer, which can enhance the fluidity of bio-based environmentally friendly asphalt and at the same time enhance the elasticity after asphalt solidification; the solid carbon particles, as part of the filler, can improve the strength and wear resistance after asphalt solidification. Selecting biomass raw materials has the characteristics of wide sources and low costs, and can also promote the recycling of organic solid wastes. In this scheme, the biomass raw materials first obtain a nitrogen mixture of gaseous biomass heavy oil and biomass hydrogen oil through pyrolysis, and the remaining solid phase is solid carbon particles. To reduce the occurrence of side reactions, the nitrogen mixture of gaseous biomass heavy oil and biomass hydrogen oil needs to be evacuated in time and gradually condensed into biomass heavy oil and biomass light oil in the follow-up. Therefore, high-temperature nitrogen needs to be introduced in step (1) to prevent the temperature of the reaction system from decreasing and making the pyrolysis reaction unstable. After the biomass light oil is condensed, the gas phase is recycled nitrogen, which still contains a small amount of light organic volatiles and can play a positive role in step (3). Therefore, except for the water consumption during the drying process, all other components of the biomass base material selected in this scheme are fully utilized.

[0014] 2. In step (2), the vaporized biomass heavy oil is introduced into the plastic substrate as a heat source to melt the plastic substrate, and a better mixing effect can be obtained. The condensed biomass heavy oil is still a high-temperature substance with a temperature of 180°C to 250°C, and only a small amount of heat energy is required to vaporize it. This makes this scheme save more energy compared with mixing liquid heavy oil into the melted plastic substrate. Since introducing biomass heavy oil into asphalt will improve the fluidity of asphalt, increase the penetration, and lower the softening temperature, in this scheme, the biomass heavy oil and the plastic substrate are mixed first to introduce the plastic substrate to reduce the penetration of the final product of bio-based environmentally friendly asphalt and increase the softening temperature. Then, recycled rubber particle materials are introduced to introduce the high elastic compressive performance of rubber, thereby improving the comprehensive performance of bio-based environmentally friendly asphalt.

[0015] 3. The intermediate products in the entire preparation process flow are not cooled down, and the remaining heat is brought into the next process until bio-based environmentally friendly asphalt is obtained. In addition to the above-mentioned recycled nitrogen, biomass heavy oil, biomass light oil, etc., the prefabricated doped material obtained in step (2) is also incorporated into step (3) at a relatively high temperature to ensure the temperature of the mixture of each component and make the mixture of each component have better fluidity. The remaining heat of the recycled nitrogen can also be further utilized in step (3).

[0016] 4. The performance characteristics of each component can be superimposed on each other, resulting in improved comprehensive performance. In step (4), heating the materials of each component to 130°C - 180°C under the condition of recycled nitrogen and then adding the prefabricated dopant can make the mixing of each component more uniform. At the same time, a small amount of biomass light oil volatiles contained in the recycled nitrogen may enter the bio-based environmentally friendly asphalt as a small amount of plasticizer. The biomass heavy oil has good compatibility with the matrix asphalt. Under the preparation conditions of step (2), the biomass heavy oil in the prefabricated dopant combines with the plastic substrate, improving the compatibility between the plastic substrate and the asphalt. The biomass light oil and solid carbon particles are pre-mixed, which can better incorporate the solid carbon particles into the prefabricated dopant, improving the fluidity of the prefabricated dopant and at the same time enhancing the wear resistance of the bio-based environmentally friendly asphalt.

[0017] Preferably, the temperature of the low-heat nitrogen in step (1) is 130°C - 180°C; the temperature of the high-heat nitrogen is 500°C - 600°C.

[0018] To ensure the temperature of drying and pyrolysis reactions, the temperature of the nitrogen introduced should be slightly higher than the drying and pyrolysis reaction temperatures, especially the pyrolysis temperature. The introduction of high-heat nitrogen can ensure the stability of the reaction.

[0019] Preferably, the gas flow rate of the high-heat nitrogen in step (1) is 1% - 5% of the total gas volume per second.

[0020] To quickly extract the pyrolysis products, it is necessary to ensure the gas flow rate of the high-heat nitrogen. Taking the total gas volume in the reaction system as unit 1, the gas flow rate is 1% - 5% of the total gas volume per second. In other words, the nitrogen in the reaction system should be completely replaced at least once per minute.

[0021] Preferably, the heating rate for quickly heating to 450°C - 550°C in step (1) is 100°C - 200°C per second.

[0022] Preferably, the temperature of the biomass heavy oil in step (1) is 180°C - 250°C; the temperature of the biomass light oil is 100°C - 180°C; the temperature of the recycled nitrogen is 90°C - 150°C.

[0023] Preferably, in step (2), the process conditions for heating and vaporizing the biomass heavy oil are: heating to 300°C - 350°C under nitrogen conditions, vaporizing to obtain biomass heavy oil vapor.

[0024] Preferably, in step (2), the preparation process of the mixture of biomass light oil and solid carbon particles is as follows: under nitrogen conditions, the solid carbon particles and biomass light oil are mixed at a weight ratio of 1:1 to 2 to obtain mixture A. After mixture A is roll-pressed and crushed, it is dispersed for 5 to 10 minutes at 800 r / min to 1000 r / min to obtain the mixture of biomass light oil and solid carbon particles.

[0025] The function of roll-pressing is to crush large solid carbon particles. This process has a certain modification effect. After roll-pressing, the solid carbon particles have better compatibility with biomass light oil and better dispersibility in the prefabricated doping material.

[0026] Preferably, in step (2), the plastic substrate is recycled bottle chips or thermoplastic plastic particles.

[0027] Preferably, in step (3), the matrix asphalt is one of petroleum asphalt, coal asphalt, and plant asphalt; the additives are one or several of antioxidants, anti-stripping agents, and pH regulators.

[0028] The antioxidant is one of phenolic antioxidants, phosphorus antioxidants, and imine antioxidants; the anti-stripping agent is one or several of monolauryl phosphate, triethanolamine, epoxy resin, acrylamide, polyvinyl alcohol fiber, and portland cement; the pH regulator is one or more of sodium carbonate, potassium carbonate, sodium hydroxide, or potassium hydroxide; the filler is one or more of calcium carbonate powder, silica powder, kaolin powder, titanium dioxide powder, and the solid carbon particles obtained in step (1).

[0029] Preferably, in step (3), the particle size of the recycled rubber particle material is less than 5 mm.

[0030] The particle size of the recycled rubber particle material should not be too large. If the particle size is too large, the recycled rubber particle material cannot be completely melted, resulting in large particles in the finally prepared bio-based environmentally friendly asphalt, which will cause a decline in mechanical properties.

[0031] Preferably, in step (3), the temperature when 3 to 5 parts of the prefabricated doping material are added after mixing evenly is 150°C to 200°C.

[0032] Ensure that the temperature of the prefabricated doping material in step (3) can ensure the temperature of the materials during the mixing process, ensure sufficient fluidity, and thus ensure uniform mixing.

[0033] This solution also provides a bio-based environmentally friendly asphalt prepared by the above preparation method.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] 1. Biomass raw materials are selected to prepare biomass heavy oil, solid carbon particles and biomass light oil as the raw and auxiliary materials for bio-based environmental protection asphalt. At the same time, recycled rubber particles are added to achieve the purpose of resource recycling;

[0036] 2. In the process system, the vaporized biomass heavy oil is introduced into the plastic substrate as a heat source to melt the plastic substrate, which can obtain a better mixing effect; the recycled nitrogen is used as a protective gas in the preparation process of bio-based environmental protection asphalt. The waste heat in biomass heavy oil, biomass light oil and recycled nitrogen is fully utilized, saving energy;

[0037] 3. In terms of the formula, the bio-based environmental protection asphalt described in this solution enhances the affinity between plastic, asphalt and rubber through biomass heavy oil, improves the fluidity of bio-based environmental protection asphalt and the dispersibility of solid carbon particles through biomass light oil, and fully combines the properties of plastic, rubber and asphalt to produce bio-based environmental protection asphalt with penetration, ductility and softening temperature suitable for most usage environments. Specific Embodiments

[0038] The following describes the preferred embodiments of the present invention. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention and are not used to limit the present invention.

[0039] Example 1

[0040] A method for preparing bio-based environmental protection asphalt includes the following steps:

[0041] Step (1): The wood processing debris is dried in a nitrogen environment at 130°C until the water content is lower than 0.5%. After being washed with low-temperature nitrogen at 150°C, it is rapidly heated to 500°C at a heating rate of 150°C per second. After reacting for 4 minutes, high-temperature nitrogen at 550°C is introduced at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. The oil-containing nitrogen is introduced into the first liquefaction tank to obtain biomass heavy oil at 230°C and light oil-containing nitrogen. The light oil-containing nitrogen is liquefied in the second liquefaction tank to obtain biomass light oil at 150°C and recycled nitrogen at 120°C;

[0042] Step (2): By weight, 10 parts of the biomass heavy oil obtained in step (1) is heated to 330°C and vaporized in a nitrogen condition. The vaporized steam is introduced into 15 parts of recycled bottle chips, and continuously stirred until the recycled bottle chips are completely melted. Then, 2 parts of the mixture of biomass light oil and solid carbon particles obtained in step (1) are added, and stirring is continued to obtain a prefabricated doped material;

[0043] The preparation process of the mixture of biomass light oil and solid carbon particles is as follows: Under nitrogen conditions, mix solid carbon particles and biomass light oil in a weight ratio of 1:1 to obtain mixture A. After roll-pressing and crushing mixture A, disperse it for 10 minutes at 900 r / min to obtain the mixture of biomass light oil and solid carbon particles;

[0044] Step (3): By weight, take 20 parts of petroleum asphalt, 7 parts of recycled rubber particle material with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1). Heat them to 150 °C under recycled nitrogen conditions, and then add 4 parts of prefabricated doping material at 160 °C. After mixing evenly, obtain the bio-based environmental protection asphalt.

[0045] Example 2

[0046] A preparation method of bio-based environmental protection asphalt includes the following steps:

[0047] Step (1): Dry the crop straw at 120 °C in a nitrogen environment until the water content is lower than 0.5%. After cleaning with low-temperature nitrogen at 130 °C, rapidly heat it to 480 °C at a heating rate of 100 °C per second. After reacting for 5 minutes, introduce high-temperature nitrogen at 500 °C at a flow rate of 2% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil at 200 °C and light oil-containing nitrogen. Pass the light oil-containing nitrogen into the second liquefaction tank for liquefaction to obtain biomass light oil at 120 °C and recycled nitrogen at 90 °C;

[0048] Step (2): By weight, heat 8 parts of the biomass heavy oil obtained in step (1) to vaporize at 300 °C under nitrogen conditions. Pass the vaporized steam into 15 parts of thermoplastic plastic particles and continuously stir until the thermoplastic plastic particles are completely melted. Then add 3 parts of the mixture of biomass light oil and solid carbon particles obtained in step (1) and continue to stir to obtain the prefabricated doping material;

[0049] The preparation process of the mixture of biomass light oil and solid carbon particles is as follows: Under nitrogen conditions, mix solid carbon particles and biomass light oil in a weight ratio of 1:1.5 to obtain mixture A. After roll-pressing and crushing mixture A, disperse it for 8 minutes at 1000 r / min to obtain the mixture of biomass light oil and solid carbon particles;

[0050] Step (3): By weight, take 15 parts of coal tar pitch, 5 to 8 parts of recycled rubber granule materials with a particle size less than 5 mm, 0.5 part of n-isopropyl-2-naphthylamine, 0.5 part of polyvinyl alcohol fiber, 0.1 part of sodium hydroxide, 1 part of silicon dioxide powder, kaolin powder, 1 part of titanium dioxide powder and 1 part of the solid carbon particles obtained in step (1), heat them to 140 °C under the condition of recycled nitrogen, then add 3 parts of prefabricated doping materials at 180 °C, and mix evenly to obtain the bio-based environmentally friendly asphalt.

[0051] Example 3

[0052] A preparation method of bio-based environmentally friendly asphalt, comprising the following steps:

[0053] Step (1): Dry the kitchen waste at 150 °C in a nitrogen environment until the water content is lower than 0.5%, wash it with low-temperature nitrogen at 180 °C, then rapidly heat it to 530 °C at a heating rate of 200 °C per second, react for 5 minutes, and then introduce high-temperature nitrogen at 580 °C at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil at 220 °C and light oil-containing nitrogen, and pass the light oil-containing nitrogen into the second liquefaction tank for liquefaction to obtain biomass light oil at 160 °C and recycled nitrogen at 130 °C;

[0054] Step (2): By weight, heat 6 parts of the biomass heavy oil obtained in step (1) to vaporize at 330 °C under the condition of nitrogen, pass the vaporized steam into 10 parts of recycled bottle chips, continuously stir until the recycled bottle chips are completely melted, then add 3 parts of the mixture of the biomass light oil and solid carbon particles obtained in step (1), and continue to stir to obtain the prefabricated doping material;

[0055] The preparation process of the mixture of biomass light oil and solid carbon particles is as follows: Under the condition of nitrogen, mix the solid carbon particles and biomass light oil in a weight ratio of 1:2 to obtain mixture A. After mixture A is roll-pressed and crushed, disperse it at 800 r / min for 10 minutes to obtain the mixture of biomass light oil and solid carbon particles;

[0056] Step (3): By weight, take 20 parts of plant asphalt, 6 parts of recycled rubber granule materials with a particle size less than 5 mm, 0.5 part of n-isopropyl-2-naphthylamine, 0.5 part of polyvinyl alcohol fiber, 1 part of silicon dioxide powder, 1 part of the solid carbon particles obtained in step (1), heat them to 170 °C under the condition of recycled nitrogen, then add 3 parts of prefabricated doping materials at 160 °C, and mix evenly to obtain the bio-based environmentally friendly asphalt.

[0057] Comparative Example 1

[0058] Step (1): 15 parts of recycled bottle chips are heated to 330 °C under nitrogen conditions and continuously stirred until the recycled bottle chips are completely melted. Subsequently, 2 parts of carbon powder are added and stirring is continued to obtain a prefabricated doping material.

[0059] Step (2): By weight, 20 parts of petroleum asphalt, 7 parts of recycled rubber granule material with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, and 1 part of silicon dioxide powder are heated to 150 °C under nitrogen conditions. Subsequently, 4 parts of the prefabricated doping material at 160 °C are added and mixed evenly to obtain a bio-based environmental protection asphalt.

[0060] Comparative Example 2

[0061] Step (1): Wood processing debris is dried in a nitrogen environment at 130 °C until the water content is less than 0.5%. After being washed with low-temperature nitrogen at 150 °C, it is heated to 500 °C at a heating rate of 50 °C per second and reacted for 4 minutes. Then, high-temperature nitrogen at 550 °C is introduced at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. The oil-containing nitrogen is introduced into the first liquefaction tank to obtain biomass heavy oil at 230 °C and light oil-containing nitrogen. The light oil-containing nitrogen is liquefied in the second liquefaction tank to obtain biomass light oil at 150 °C and recycled nitrogen at 120 °C.

[0062] Step (2): By weight, 10 parts of the biomass heavy oil obtained in step (1) are vaporized by heating to 330 °C under nitrogen conditions. The vaporized vapor is introduced into 15 parts of recycled bottle chips and continuously stirred until the recycled bottle chips are completely melted. Subsequently, 2 parts of the mixture of biomass light oil and solid carbon particles obtained in step (1) are added and stirring is continued to obtain a prefabricated doping material.

[0063] The preparation process of the mixture of biomass light oil and solid carbon particles is as follows: Under nitrogen conditions, they are mixed in a weight ratio of solid carbon particles to biomass light oil of 1:1 to obtain mixture A. After mixture A is roll-pressed and crushed, it is dispersed at 900 r / min for 10 minutes to obtain the mixture of biomass light oil and solid carbon particles.

[0064] Step (3): By weight, 20 parts of petroleum asphalt, 7 parts of recycled rubber granule material with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1) are heated to 150 °C under recycled nitrogen conditions. Subsequently, 4 parts of the prefabricated doping material at 160 °C are added and mixed evenly to obtain a bio-based environmental protection asphalt.

[0065] Comparative Example 3

[0066] A preparation method of a biological environmental protection type asphalt, comprising the following steps:

[0067] Step (1): Process the wood processing debris at 130 °C in a nitrogen environment until the water content is lower than 0.5%. After cleaning with low-temperature nitrogen at 150 °C, rapidly heat it to 500 °C at a heating rate of 150 °C per second. After reacting for 10 minutes, introduce high-temperature nitrogen at 550 °C continuously at a flow rate of 0.5% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil at 230 °C and light oil-containing nitrogen. After liquefying the light oil-containing nitrogen in the second liquefaction tank, obtain biomass light oil at 150 °C and recycled nitrogen at 120 °C;

[0068] Step (2): By weight, heat 10 parts of the biomass heavy oil obtained in step (1) to vaporize at 330 °C in a nitrogen condition. Pass the vaporized vapor into 15 parts of recycled bottle chips, and continuously stir until the recycled bottle chips are completely melted. Subsequently, add 2 parts of the mixture of biomass light oil and solid carbon particles obtained in step (1), and continue to stir to obtain a prefabricated doping material;

[0069] The preparation process of the mixture of biomass light oil and solid carbon particles is as follows: Under nitrogen conditions, mix the solid carbon particles and biomass light oil in a weight ratio of 1:1 to obtain mixture A. After roll-pressing and crushing mixture A, disperse it at 900 r / min for 10 minutes to obtain the mixture of biomass light oil and solid carbon particles

[0070] Step (3): By weight, heat 20 parts of petroleum asphalt, 7 parts of recycled rubber particle materials with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1) to 150 °C under recycled nitrogen conditions. Subsequently, add 4 parts of the prefabricated doping material at 160 °C, and mix evenly to obtain the biological environmental protection type asphalt.

[0071] Comparative Example 4

[0072] Step (1): Process the wood processing debris at 130 °C in a nitrogen environment until the water content is lower than 0.5%. After cleaning with low-temperature nitrogen at 150 °C, rapidly heat it to 500 °C at a heating rate of 150 °C per second. After reacting for 4 minutes, introduce continuous nitrogen at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil at 230 °C and light oil-containing nitrogen. After liquefying the light oil-containing nitrogen in the second liquefaction tank, obtain biomass light oil at 150 °C and recycled nitrogen at 120 °C;

[0073] Step (2): By weight, heat 10 parts of the biomass heavy oil obtained in step (1) to 330 °C for vaporization under nitrogen conditions, and introduce the vaporized steam into 15 parts of recycled bottle chips. Continuously stir until the recycled bottle chips are completely melted, and then add 2 parts of the mixture of biomass light oil and solid carbon particles obtained in step (1). Continue stirring to obtain a prefabricated doping material;

[0074] The preparation process of the mixture of biomass light oil and solid carbon particles is as follows: Under nitrogen conditions, mix the solid carbon particles and biomass light oil in a weight ratio of 1:1 to obtain mixture A. After roller pressing and crushing mixture A, disperse it at 900 r / min for 10 min to obtain the mixture of biomass light oil and solid carbon particles;

[0075] Step (3): By weight, mix 20 parts of petroleum asphalt, 7 parts of recycled rubber particle material with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1). Heat it to 150 °C under recycled nitrogen conditions, and then add 4 parts of the prefabricated doping material at 160 °C. Mix evenly to obtain a bio-based environmental protection asphalt.

[0076] Comparative Example 5

[0077] Step (1): Dry the wood processing debris in a nitrogen environment at 130 °C until the water content is less than 0.5%. After cleaning with low-heat nitrogen at 150 °C, rapidly heat it to 500 °C at a heating rate of 150 °C per second. After reacting for 4 min, introduce high-heat nitrogen at 550 °C continuously at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into a liquefaction tank to obtain biomass oil at 230 °C and recycled nitrogen;

[0078] Step (2): By weight, heat 10 parts of the biomass oil obtained in step (1) to 330 °C for vaporization under nitrogen conditions, and introduce the vaporized steam into 15 parts of recycled bottle chips. Continuously stir until the recycled bottle chips are completely melted, and then add 2 parts of the mixture of biomass oil and solid carbon particles obtained in step (1). Continue stirring to obtain a prefabricated doping material;

[0079] The preparation process of the mixture of biomass oil and solid carbon particles is as follows: Under nitrogen conditions, mix the solid carbon particles and biomass oil in a weight ratio of 1:1 to obtain mixture A. After roller pressing and crushing mixture A, disperse it at 900 r / min for 10 min to obtain the mixture of biomass light oil and solid carbon particles;

[0080] Step (3): By weight, take 20 parts of petroleum asphalt, 7 parts of recycled rubber granule material with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1). Heat them to 150 °C under the condition of recycled nitrogen, and then add 4 parts of prefabricated doping material at 160 °C. After mixing evenly, a bio-based environmentally friendly asphalt is obtained.

[0081] Comparative Example 6

[0082] Step (1): Dry the wood processing debris in a nitrogen environment at 130 °C until the water content is lower than 0.5%. After cleaning with low-temperature nitrogen at 150 °C, rapidly heat it to 500 °C at a heating rate of 150 °C per second. After reacting for 4 minutes, introduce high-temperature nitrogen at 550 °C at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil at 230 °C and light oil-containing nitrogen. Pass the light oil-containing nitrogen into the second liquefaction tank for liquefaction to obtain biomass light oil at 150 °C and recycled nitrogen at 120 °C;

[0083] Step (2): By weight, cool 10 parts of the biomass heavy oil obtained in step (1) and mix it with 15 parts of recycled bottle flakes. Then heat it to 330 °C and continuously stir until the recycled bottle flakes are completely melted. Then add 2 parts of the mixture of cooled biomass light oil and solid carbon particles obtained in step (1), and continue to stir to obtain the prefabricated doping material;

[0084] The preparation process of the mixture of cooled biomass light oil and solid carbon particles is as follows: Under the condition of nitrogen, mix the solid carbon particles and cooled biomass light oil in a weight ratio of 1:1 to obtain mixture A. After roll-pressing and crushing mixture A, disperse it at 900 r / min for 10 minutes to obtain the mixture of biomass light oil and solid carbon particles.

[0085] Step (3): By weight, take 20 parts of petroleum asphalt, 7 parts of recycled rubber granule material with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1). Heat them to 150 °C under the condition of recycled nitrogen, and then add 4 parts of prefabricated doping material at 160 °C. After mixing evenly, a bio-based environmentally friendly asphalt is obtained.

[0086] Comparative Example 7

[0087] A preparation method of a bio-based environmentally friendly asphalt, comprising the following steps:

[0088] Step (1): Dry the wood processing debris at 130°C in a nitrogen environment until the water content is less than 0.5%. After cleaning with low-temperature nitrogen at 150°C, rapidly heat it to 500°C at a heating rate of 150°C per second. After reacting for 4 minutes, introduce high-temperature nitrogen at 550°C continuously at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil at 230°C and light-oil-containing nitrogen. After liquefying the light-oil-containing nitrogen in the second liquefaction tank, obtain biomass light oil at 150°C and recycled nitrogen at 120°C;

[0089] Step (2): By weight, heat 10 parts of the biomass heavy oil obtained in step (1) to vaporize at 330°C in a nitrogen condition, and pass the vaporized steam into 15 parts of recycled bottle chips, and continuously stir until the recycled bottle chips are completely melted to obtain a prefabricated doping material;

[0090] Step (3): By weight, mix 20 parts of petroleum asphalt, 7 parts of recycled rubber particle materials with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1). Heat them to 150°C under the condition of recycled nitrogen, and then add 4 parts of the prefabricated doping material at 160°C, and mix evenly to obtain a bio-based environmentally friendly asphalt.

[0091] Comparative Example 8

[0092] A preparation method of a bio-based environmentally friendly asphalt, comprising the following steps:

[0093] Step (1): Dry the wood processing debris at 130°C in a nitrogen environment until the water content is less than 0.5%. After cleaning with low-temperature nitrogen at 150°C, rapidly heat it to 500°C at a heating rate of 150°C per second. After reacting for 4 minutes, introduce high-temperature nitrogen at 550°C continuously at a flow rate of 3% of the total gas volume per second to obtain oil-containing nitrogen and solid carbon particles. Pass the oil-containing nitrogen into the first liquefaction tank to obtain biomass heavy oil at 230°C and light-oil-containing nitrogen. After liquefying the light-oil-containing nitrogen in the second liquefaction tank, obtain biomass light oil at 150°C and recycled nitrogen at 120°C;

[0094] Step (2): By weight, mix 20 parts of petroleum asphalt, 7 parts of recycled rubber particle materials with a particle size less than 5 mm, 1 part of calcium hydrogen phosphate, 0.5 part of monolauryl phosphate, 0.1 part of sodium carbonate, 1 part of calcium carbonate powder, 1 part of silicon dioxide powder, and 1 part of the solid carbon particles obtained in step (1). Heat them to 150°C under the condition of recycled nitrogen, and then add 4 parts of the biomass heavy oil at 160°C, and mix evenly to obtain a bio-based environmentally friendly asphalt.

[0095] Detection method:

[0096] 1. Penetration: At a temperature of 25°C, using a standard needle of 100 grams, the depth (in 1 / 10 mm) that the needle vertically penetrates into the asphalt sample within 5 seconds. The higher the penetration value, the softer the asphalt and the lower its viscosity.

[0097] 2. Ductility: Measured by a ductility tester under standard conditions (25°C, stretching speed of 5 cm / min), the elongation length (in cm) when the asphalt sample breaks. The larger the ductility value, the stronger the plasticity of the asphalt.

[0098] 3. Softening point: Tested by the ring-and-ball method. The asphalt sample is placed in a copper ring of specific dimensions (diameter 16 mm, height 6 mm), a standard steel ball is placed on the sample, and then heated at a specified rate (5°C / min) until the asphalt softens. The higher the softening point, the better the heat resistance of the asphalt.

[0099] Table 1 Test and Comparison Results

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[0102] Since the performance of asphalt is closely related to the use environment, geography, and climate, it is impossible to directly evaluate the performance of Examples 1 - 3 and Comparative Examples 1 - 7. However, from the results, Examples 1 - 3 can be applied to most regions. In Comparative Example 1, Comparative Example 4, and Comparative Example 6, the ductility is low and it is prone to cracking, so they may not be suitable for use in low-temperature regions and high-load roads; in Comparative Example 2, Comparative Example 3, Comparative Example 5, Comparative Example 7, and Comparative Example 8, the softening temperature is low, so they may not be suitable for use in high-temperature places.

[0103] The difference between Comparative Example 1 and Example 1 is that biomass raw materials were not selected. In Comparative Example 1, the bottle chips were directly heated to melt and added to the base asphalt in step (3). The compatibility between the bottle chips and the base asphalt is worse than that in Example 1, resulting in poorer ductility. It may be that the bottle chip molecules hinder the movement of the base asphalt molecules, and crack sources are formed at the contact positions between the bottle chip molecular clusters and the base asphalt molecular clusters. This may also be the reason for the high softening temperature.

[0104] The difference between Comparative Example 2 and Example 1 is that in step (1), after vaporization, it was introduced into 15 parts of recycled bottle chips at a heating rate of 50°C per second. The too-slow heating rate led to side reactions, and then to too low a softening temperature point and too large a penetration depth; the difference between Comparative Example 3 and Example 1 is that in step (1), it was quickly heated to 500°C, and after reacting for 10 minutes, high-temperature nitrogen at 550°C was introduced at a flow rate of 0.5% of the total gas volume per second. This comparative example also had more side reactions, resulting in side reactions and then too low a softening temperature point and too large a penetration degree.

[0105] The difference between Comparative Example 4 and Example 1 is that in step (1), nitrogen gas is introduced at a flow rate of 3% of the total gas volume per second, instead of high-temperature nitrogen gas. This makes it necessary to reheat the nitrogen gas introduced into the reaction system, increasing the difficulty of temperature control, resulting in a decrease in product stability, an increase in hardness, an increase in softening temperature, and a decrease in ductility. The difference between Comparative Example 6 and Example 1 is that in step (2), 10 parts of the biomass heavy oil obtained in step (1) is cooled and then mixed with 15 parts of recycled bottle chips. That is, the biomass heavy oil is not vaporized and used as a heat source and a component, but simply mixed with the recycled bottle chips in the form of a component. Since the bottle chips are relatively thin, they may overlap with each other, resulting in uneven distribution of the biomass heavy oil, and thus also causing large fluctuations in the product, an increase in hardness, an increase in softening temperature, and a decrease in ductility.

[0106] The difference between Comparative Example 5 and Example 1 is that it is not divided into biomass heavy oil and biomass light oil, and only biomass oil is incorporated into the subsequent process. In Comparative Example 5, the proportion of biomass light oil is too high, resulting in large penetration and ductility, that is, the product is relatively soft. However, the problem is that the softening temperature is low and it cannot be used in summer in the south.

[0107] The difference between Comparative Example 7 and Example 1 is that in step (2), the mixture of cooled biomass light oil and solid carbon particles is not prepared and not selected. In step (2) of Example 1, the solid carbon particles are equivalent to a part of the filler. After being made into a mixture with the biomass light oil, they can be better dispersed in the plastic substrate and biomass heavy oil in step (2), and then can be better dispersed in the whole component subsequently. The non-selection in Comparative Example 7 results in an increase in penetration and an increase in ductility.

[0108] The difference between Comparative Example 8 and Example 1 is that no plastic substrate is added. It can be seen from Comparative Example 8 that the biomass heavy oil improves the fluidity of the asphalt, increases the penetration, increases the ductility, but decreases the softening temperature.

[0109] In addition, Examples 1-3 make full use of the waste heat in the biomass heavy oil, biomass light oil, and recycled nitrogen gas. Compared with the prior art, that is, some of the above comparative examples, such as Comparative Example 6, etc., it has greater energy-saving advantages in long-term production.

[0110] The above is only the preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution of the present invention and its inventive concept, makes equivalent substitutions or changes, and should be covered by the protection scope of the present invention.

Claims

1. A method for preparing bio-based environmentally friendly asphalt, characterized in that: The following steps are involved: Step (1): drying the biomass raw material at 120°C to 150°C in a nitrogen environment until the water content is less than 0.5%, washing with low-heat nitrogen, rapidly heating to 450°C to 550°C, reacting for 3min to 5min, introducing continuous high-heat nitrogen to obtain oil-containing nitrogen and solid carbon particles, introducing the oil-containing nitrogen into a first liquefaction tank to obtain biomass heavy oil and light oil-containing nitrogen, introducing the light oil-containing nitrogen into a second liquefaction tank for liquefaction to obtain biomass light oil and recovered nitrogen; the temperature of the high-heat nitrogen is 500°C to 600°C; the gas flow rate of the high-heat nitrogen is 1% to 5% of the total gas volume per second; Step (2): by weight, 5 to 10 parts of the biomass heavy oil obtained in step (1) are heated and vaporized, and then introduced into 10 to 20 parts of a plastic substrate, and stirred continuously until the plastic substrate is completely melted, and then 1 to 3 parts of a mixture of the biomass light oil obtained in step (1) and solid carbon particles are added, and stirring is continued to obtain a prefabricated doping material; Step (3): by weight, 10 to 20 parts of base asphalt, 5 to 8 parts of recycled rubber particles, 0.1 to 2 parts of additives and 1 to 3 parts of fillers are heated to 130°C to 180°C under the condition of recycled nitrogen, and then 3 to 5 parts of prefabricated doping materials are added and mixed evenly to obtain bio-based environmentally friendly asphalt.

2. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: The temperature of the low-heat nitrogen in step (1) is 130°C to 180°C; the temperature of the biomass heavy oil in step (1) is 180°C to 250°C; the temperature of the biomass light oil is 100°C to 180°C; and the temperature of the recovered nitrogen is 90°C to 150°C.

3. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: The heating rate of the rapid heating to 450°C to 550°C in step (1) is 100°C to 200°C per second.

4. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: In step (2), the process conditions for heating and vaporizing the biomass heavy oil are: heating to 300° C. to 350° C. under nitrogen conditions, vaporizing, and obtaining biomass heavy oil vapor.

5. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: In step (2), the preparation process of the mixture of biomass light oil and solid carbon particles is as follows: under nitrogen conditions, solid carbon particles and biomass light oil are mixed in a weight ratio of 1:1 to 2 to obtain a mixture A; after the mixture A is roller-crushed, it is dispersed at 800 r / min to 1000 r / min for 5 min to 10 min to obtain a mixture of biomass light oil and solid carbon particles.

6. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: In step (2), the plastic substrate is recycled bottle flakes or thermoplastic plastic particles.

7. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: In step (3), the matrix asphalt is one of petroleum asphalt, coal asphalt, and plant asphalt; the auxiliary agent is one or more of an antioxidant, an anti-stripping agent, and a pH adjuster; the filler is one or more of calcium carbonate powder, silicon dioxide powder, kaolin powder, titanium dioxide powder, and the solid carbon particles obtained in step (1).

8. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: In step (3), the particle size of the recycled rubber particles is less than 5 mm.

9. The method for preparing the bio-based environmentally friendly asphalt according to claim 1, characterized in that: In step (3), the temperature of adding 3 to 5 parts of prefabricated doping materials after mixing evenly is 150°C to 200°C.

10. A bio-based environmentally friendly asphalt prepared by the method for preparing the bio-based environmentally friendly asphalt as claimed in any one of claims 1 to 9.

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