CN113560319B - Solvent gasification pyrolysis device and method for waste circuit board - Google Patents
Solvent gasification pyrolysis device and method for waste circuit board Download PDFInfo
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- CN113560319B CN113560319B CN202110826551.3A CN202110826551A CN113560319B CN 113560319 B CN113560319 B CN 113560319B CN 202110826551 A CN202110826551 A CN 202110826551A CN 113560319 B CN113560319 B CN 113560319B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/009—Collecting, removing and/or treatment of the condensate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/12—Applying additives during coking
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/14—Features of low-temperature carbonising processes
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- G—PHYSICS
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- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/26—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
- G01M3/32—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators
- G01M3/3236—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers
- G01M3/3272—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers for verifying the internal pressure of closed containers
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]
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Abstract
The invention relates to the technical field of comprehensive recycling of solid waste resources. The solvent gasification pyrolysis device for the waste circuit board comprises a pyrolysis reactor and a solvent gasification device, wherein the pyrolysis reactor is sequentially communicated with a condensing box, an oil tank, a condensing pipe, a solvent tank, a two-stage alkali washing tank, an activated carbon adsorption tank and a gas collecting device; the solvent gasification device is provided with an air inlet, a liquid inlet and an air outlet; the gas outlet is communicated with one end of the gas inlet pipe; the gas inlet pipe is communicated with the pyrolysis reactor; the gas inlet is communicated with an inert gas bottle through a pipeline; the liquid inlet is communicated with a solvent pump and a solvent tank in sequence; and a material reaction device is arranged in the pyrolysis reactor. The invention can effectively separate metal and nonmetal substances in the waste circuit board, has obvious effect of degrading organic components of the waste circuit board, can obviously reduce the content of pollutants in the pyrolysis product, improves the utilization rate of the pyrolysis product, and has good application prospect.
Description
Technical Field
The invention relates to the technical field of comprehensive recycling of solid waste resources, in particular to a solvent gasification low-temperature pyrolysis device and method for a waste circuit board.
Background
With the rapid development of the electronic industry and the information industry, the updating period of electronic products is continuously shortened, and the yield of electronic wastes is gradually increased. The waste circuit board is an important component in electronic waste and is composed of metal, organic resin and reinforcing materials, wherein the organic resin is used as an adhesive to combine the metal and the reinforcing materials, and common organic resin comprises phenolic resin, epoxy resin and the like. The recycling of high-value components (metal, plastic and the like) of the waste circuit board has great economic value, but the existence of heavy metal elements and brominated flame retardants makes the resource treatment process of the waste circuit board difficult to realize the synergistic development of circular economy and ecological environment. The conventional disposal methods of the waste circuit board include a burning method, a leaching method, a mechanical crushing method and the like. The incineration method removes the plastic on the waste circuit board through combustion, so that valuable metals are fully dissociated, but in an oxygen environment, due to the addition of halogen elements (Br) in the plastic and the catalytic action of metallic copper, a large amount of dioxin is easily generated in the incineration process of the waste circuit board, and serious environmental pollution is caused. The leaching method is used for dissolving and refining valuable metals on the waste circuit board through acid/alkaline solution, so that a large amount of waste liquid is generated while valuable metal components are efficiently recovered, and the environmental hazard is caused. The mechanical crushing method crushes the waste circuit boards into extremely small particles through mechanical force, separates metal and nonmetal particles through a physical sorting method, and recovers valuable metal components, but has the problems of incomplete dissociation and high energy consumption. The traditional resource utilization technology of the waste circuit board has the problems of high energy consumption, great environmental pollution and the like, and cannot realize comprehensive recycling of non-metal components.
Application number 201420080674.2 discloses a old and useless printed circuit board pyrolysis debromination device, and the device includes pyrolysis furnace body, absorption catalytic unit, spiral condensing equipment, liquid collection device, water seal arrangement, separator and tail gas processing apparatus, abandonmentThe pyrolysis gas after the circuit board pyrolysis enters an adsorption catalytic device for debromination, and adsorption catalytic substances used in the adsorption catalytic device are in a granular form and comprise FeOOH and active Al2O3Particles, HZSM-5. However, the adsorption catalyst of the method is difficult to convert organic bromine into inorganic bromine, and the adsorption catalyst is easy to adsorb organic compounds, so that the yield of pyrolysis liquid and gas products is reduced, and the adsorption catalyst is difficult to reuse, thereby causing waste of resources.
Application number 201410619847.8 discloses a water vapor gasification separation device and method for waste printed circuit boards, wherein molten salt is added into a reaction furnace, the reaction temperature is controlled at 600-700 ℃, so that organic matters of the waste printed circuit boards are rapidly pyrolyzed in a molten salt bath, and coke generated by pyrolysis and water vapor are subjected to water gas reaction to generate hydrogen and carbon dioxide by adding water vapor into a reaction system. The method adopts a molten salt co-pyrolysis method to fix bromine in the molten salt, so that the bromine-containing molten salt and a pyrolysis solid product are difficult to separate, and the cost and the environmental risk of metal recovery in subsequent molten pool smelting are increased; and the water vapor is difficult to ionize in a low-temperature system, cannot be used as a good hydrogen donor, and cannot improve the product quality of a pyrolysis liquid product.
The pyrolysis method is a promising method for completely recycling and disposing the waste circuit board resources, heating is carried out under the oxygen-free/oxygen-deficient condition, the organic components in the waste circuit board are broken after absorbing enough energy, and solid phase, liquid phase and gas phase products are formed after condensation. The solid-phase product of the waste circuit board is completely dissociated from metal and nonmetal due to the thermal decomposition of the binder; the liquid phase product has the potential of being used as chemical raw materials, clean fuels and modified products; the gas phase product can be subjected to heat value recovery and clean combustion energy supply. However, the pyrolysis liquid phase product has complex components, wide boiling range, poor flow property, high halogen content and unsatisfactory combustion performance, and the use value of the pyrolysis liquid phase product is limited, so how to effectively dehalogenate and lighten the pyrolysis liquid phase product to meet the requirements of high-quality chemical raw materials and fuel oil is always a difficult problem in the pyrolysis recovery process of waste circuit boards at present.
Disclosure of Invention
The invention aims to provide a solvent gasification low-temperature pyrolysis device and method for a waste circuit board, which are used for realizing resource recovery and harmless treatment of the waste circuit board.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a solvent gasification pyrolysis device for a waste circuit board is characterized by comprising a pyrolysis reactor and a solvent gasification device, wherein the pyrolysis reactor is sequentially communicated with a condensing box, an oil tank, a condensing pipe, a solvent tank, an alkali washing tank, an adsorption box and a gas collection device; the solvent gasification device is provided with an air inlet, a liquid inlet and an air outlet; the gas outlet is communicated with one end of the gas inlet pipe; the gas inlet pipe is communicated with the pyrolysis reactor; the gas inlet is communicated with an inert gas bottle through a pipeline; the liquid inlet is communicated with a solvent pump and a solvent tank in sequence;
and a material reaction device is arranged in the pyrolysis reactor.
Preferably, a solvent evaporation device is arranged outside the oil tank.
Preferably, the pyrolysis reactor is internally provided with a furnace shell, a heat insulation layer and a furnace body from outside; the furnace shell is provided with a No. 2 temperature control thermocouple which sequentially penetrates through the furnace shell and the heat insulation layer and is abutted against the furnace body; a silicon carbide rod is arranged between the furnace body and the heat-insulating layer;
the pyrolysis reactor is also provided with a No. 2 air inlet and an air outlet pipe; the gas inlet pipe is communicated with the pyrolysis reactor through a No. 2 gas inlet; the gas outlet pipe sequentially penetrates through the furnace shell, the heat insulation layer and the furnace body and is communicated with the hearth;
a T-shaped furnace cover and a temperature thermocouple penetrating through a central shaft of the T-shaped furnace cover are arranged above the furnace body; a sealing ring fixedly connected with the T-shaped furnace cover, a water cooling sleeve arranged between the T-shaped furnace cover and the furnace shell and a furnace cover heat preservation layer connected with the furnace body are sequentially arranged below the T-shaped furnace cover;
the pyrolysis reactor is also provided with a temperature controller connected with the silicon carbide rod, the temperature thermocouple, the No. 2 temperature control thermocouple and the air outlet pipe heat-insulating electric jacket.
Preferably, a furnace cover handle is further arranged above the T-shaped furnace cover.
Preferably, the T-shaped furnace cover is a lifting-pulling T-shaped furnace cover.
Preferably, the outlet pipe is inclined downwards.
The gas outlet pipe of the pyrolysis reactor is inclined downwards, the pyrolysis volatile matters of the waste circuit board can rapidly pass through the gas outlet pipe by utilizing the gravitational force and the driving force of the flowing gas of the system, the retention time of the pyrolysis volatile matters in the gas outlet pipe is reduced, the heavy polymerization and the polycondensation of the volatile matters are inhibited, and the product value is improved.
Preferably, the gas outlet pipe of the pyrolysis reactor is inclined at an angle of 15-30 ° to the horizontal plane.
Preferably, the outer side of the air outlet pipe outside the heat-preservation layer is provided with an air outlet pipe heat-preservation electric heating sleeve; the outlet pipe converter is arranged at the port of the outlet pipe.
The gas outlet pipe is provided with a gas outlet pipe heat-insulating electric heating sleeve, which is beneficial to preventing condensation of pyrolysis volatile matters and blocking of pipelines, and reducing the influence of test materials on the reaction device.
Preferably, the material reaction device comprises a plurality of layers of storage steel frames and fixed movable buckles, the storage steel frames are connected through the fixed movable buckles, and material frame handles are arranged on the fixed steel plates.
Preferably, the object placing steel frame is provided with a detachable crucible.
The invention also claims the pyrolysis reactor and the application of the pyrolysis reactor in a pyrolysis system.
Preferably, the condensing tank adopts a multi-stage split-flow condensing system.
The condensing box adopts a shunting condensing system, quickly condenses and pyrolyzes volatile matters, separates a pyrolysis liquid phase and a gas phase product, and has the characteristics of high separation efficiency, energy conservation, large treatment capacity, simple equipment and the like.
Preferably, the heat preservation layer is made of 1600M type high-quality high-purity alumina polycrystalline fiber, and is good in heat preservation performance and stable in structure.
Preferably, the furnace body is made of high-quality carbon steel, the inner wall is precisely polished, the outer wall is subjected to wire drawing treatment, and the corrosion resistance is good.
Preferably, 8 precise silicon carbide rods are adopted as the silicon carbide rods, the surface load is high, the oxidation resistance is good, the silicon carbide rods are uniformly distributed between the heat preservation layer and the furnace body in a circumferential shape, and the furnace body is guaranteed to be uniformly heated.
Preferably, the No. 2 temperature control thermocouple adopts a precision thermocouple, and has good stability and high precision.
Preferably, the temperature controller has a multi-section temperature control program, can set temperature rise, heat preservation and temperature reduction programs, has a PID control function, is high in control precision and small in fluctuation rate, and realizes precise control of temperature.
Preferably, the alkaline washing tank is a two-stage alkaline washing tank.
Preferably, the adsorption tank is an activated carbon or diatom ooze adsorption tank.
The invention also provides a method for pyrolyzing the waste circuit board by using the equipment, which comprises the following steps:
(1) adding the waste circuit board into the pyrolysis reactor, sealing, checking the air tightness in the pyrolysis reactor, and introducing inert gas into the solvent gasification device and the pyrolysis reactor through a gas inlet pipe to enable the atmosphere in the solvent gasification device and the pyrolysis reactor to be oxygen-free;
(2) when the atmosphere in the solvent gasification device and the pyrolysis reactor is oxygen-free, the gas flow meter is adjusted to control the flow of the inert gas to be 100-plus-200 mL/min, the temperature in the solvent gasification device is controlled to be 100-plus-200 ℃ by adjusting the setting program of the temperature controller, the temperature of the gas heat-insulating electric heating sleeve is controlled to be 100-plus-200 ℃, the temperature rise rate in the pyrolysis reactor is controlled to be 10-20 ℃/min, the final temperature of pyrolysis is controlled to be 500-plus-700 ℃, the heat-insulating time is controlled to be 0.5-2h, the temperature of the heat-insulating electric heating sleeve of the air outlet pipe is controlled to be 250-plus-300 ℃, and the temperature of the solvent evaporation device is controlled to be 100-plus-200 ℃. Wherein, the set temperature of the solvent gasification device, the gas heat-preservation electric heating jacket and the solvent evaporation device is determined according to the boiling point of the selected solvent;
(3) when the temperature thermocouple shows that the target temperature in the pyrolysis reactor reaches 200 ℃, starting a solvent pump to extract the solvent in the solvent tank, controlling the flow rate of the solvent to be 100 plus 200mL/min, gasifying the solvent into a gasifying agent through a solvent gasifying device, mixing the gasifying agent with inert carrier gas, and introducing the gasifying agent to the bottom of the pyrolysis reactor through a gas inlet pipe;
in the pyrolysis process, organic components of the waste circuit board react with a gasifying agent and are separated into a pyrolysis liquid phase product and a gas phase product through a multi-stage condensing box, the condensed pyrolysis liquid phase product is collected through an oil tank, the pyrolysis liquid phase product extracts redundant solvent through a solvent evaporation device, and the redundant solvent flows into a solvent tank to be recycled in the whole system; and removing waste gas from the pyrolysis gas-phase product through an alkaline washing tank and an adsorption box, and collecting and using the pyrolysis gas-phase product through a gas collecting device.
Preferably, in the step (1), the inert gas introduced into the solvent gasification device and the pyrolysis reactor is nitrogen.
Further, in the step (2), the temperature of the solvent gasification device, the temperature of the gas heat-preservation electric heating jacket and the temperature of the solvent evaporation device are kept consistent.
Further, in the step (3), the solvent is one or more of ethanol, n-propanol, isopropanol, n-butanol and isobutanol.
Preferably, the flow rate of the solvent is controlled by a solvent pump, and the molar ratio of the gasifying agent to the carrier gas is controlled to be 1: 1-10: 1.
Within this range, the safety and cost performance are both satisfied.
The invention is further explained below:
the pyrolysis reactor needs to be subjected to air tightness inspection after being sealed, a differential pressure type air tightness leak detector is adopted for detection, nitrogen is introduced after an air outlet valve of the pyrolysis reactor is closed, when the pressure is increased to 1Mpa, the pressure is stabilized for 20min, the pressure change condition is detected, the air tightness of the pyrolysis reactor is qualified when the pressure drop is less than or equal to 0.01Mpa, and if leakage occurs, the sealing condition of each interface of the pyrolysis reactor needs to be inspected.
The pyrolysis reactor is additionally provided with the water cooling jacket, the water cooling jacket enables the pyrolysis reactor to keep good air tightness under a high-temperature state, the sealing part of the pyrolysis reactor without the water cooling jacket is easy to be subjected to thermal expansion deformation in the pyrolysis reaction process at the temperature of more than 300 ℃, so that the sealing performance of the pyrolysis reactor is poor, the service life of the pyrolysis reactor is directly shortened, and the temperature of the sealing part of the pyrolysis reactor is in a low-temperature state through the heat exchange effect of flowing water, so that the sealing performance of the pyrolysis reactor is ensured.
The flow of the inert gas is controlled at 100-200mL/min, so that the container is kept in an oxygen-free environment at a low inert gas flow rate, the retention time of the gasifying agent is long, and the gasifying agent is prevented from being blown out of the pyrolysis reactor by the inert gas without reaction. The gas inlet pipe is introduced to the bottom of the pyrolysis reactor, so that the gasification agent is in full contact with the raw materials. The flow rate of the solvent is controlled to be 100-200mL/min, which is beneficial to controlling the content of the gasification agent in a proper range. Too large or too small is not favorable for optimal reaction. The gas outlet pipe of the pyrolysis reactor is provided with the gas outlet pipe heat-insulating electric heating sleeve, the temperature is controlled to be 250-plus-300 ℃, the gas outlet pipe heat-insulating electric heating sleeve can prevent pyrolysis volatile matters of the waste circuit board from being condensed in the gas outlet pipe, the condensation point of the volatile matters is different according to the pyrolysis process and the waste circuit board raw materials, but the condensation point of most of the volatile matters is lower than 250-plus-300 ℃, the temperature control protects smooth circulation of the gas outlet pipe, and the phenomenon of scaling and blockage in the gas outlet pipe is prevented. Meanwhile, the temperature in the pyrolysis reactor can be guaranteed to be stable only by adding the water cooling sleeve on the basis of guaranteeing sealing, and the temperature of the air outlet pipe is stabilized by matching with the heat-insulating electric heating sleeve of the air outlet pipe.
The temperature of the solvent gasification device is set according to different solvent boiling points, so that the solvent is gasified to be in a gas state, namely a gasification agent. The temperature of the gas heat-preservation electric heating jacket is set to ensure that the gasifying agent is not condensed and is safely and efficiently conveyed to the pyrolysis reactor in a gas state. The temperature of the solvent evaporation device is set according to the boiling point of the solvent, so that the solvent and the pyrolysis liquid product are effectively separated. The purpose of the solvent gasification device, the gas heat-insulating electric heating jacket and the solvent evaporation device is to keep the solvent in a gas state, and the three devices are required to keep consistent temperature.
The solvent is one or more of ethanol, normal propyl alcohol, isopropanol, normal butanol and isobutanol, the solvent gasification agent has good in-situ hydrogen supply capability in the low-temperature pyrolysis process of the waste circuit board, heavy polymerization and polycondensation of depolymerization products are effectively inhibited, the pyrolysis liquid phase product is lightened, organic bromine is effectively converted into inorganic bromine, removal of bromine in the waste circuit board is facilitated, and the solvent gasification pyrolysis principle is shown in figure 5.
One or more gasifying agents of ethanol, normal propyl alcohol, isopropyl alcohol, normal butyl alcohol and isobutyl alcohol can be used as a hydrogen donor in the pyrolysis process, hydrogen free radicals are easy to form, and the hydrogen supplying capability is excellent. Most of organic components in the waste circuit board are high polymers of brominated epoxy resin and phenolic resin, on one hand, hydrogen radicals are easy to attack Ar-Br bonds in the resin and products to form HBr, so that organic bromine is easy to be converted into inorganic bromine, the chemical property of pyrolysis products is improved, and the environment-friendly utilization of the pyrolysis products of the waste circuit board is facilitated; on the other hand, the hydrogen free radicals can inhibit the heavy polymerization and polycondensation reaction of the depolymerization products, reduce the generation of coke, greatly improve the yield of the phenol monomers, lighten the pyrolysis liquid product, improve the flow property of the liquid product and facilitate the resource utilization of the pyrolysis product.
The material reaction device adopts a multi-stage object placing steel frame, the detachable crucibles are embedded in the multi-stage object placing steel frame, the height of each crucible is half of that of each stage of object placing steel frame, and the arrangement of the height of each crucible is favorable for the material exchange between the raw material pyrolysis process and the gasifying agent. The multistage supporter set up the area of contact that has increased waste circuit board raw materials and pyrolysis volatile and gasification agent for the reaction is more abundant thorough.
Compared with the prior art, the invention has the advantages that:
(1) the solvent gasification low-temperature pyrolysis method for the waste circuit board adopts a solvent circulation process, realizes the recycling of the solvent in the low-temperature pyrolysis process of the waste circuit board through a 'gasification-condensation-solvent separation-condensation' circulation mode, has no secondary pollution, fully utilizes resources and has excellent treatment effect; and the whole solvent circulation process is completed in an inert atmosphere, so that the safety performance is improved.
(2) According to the solvent gasification low-temperature pyrolysis method for the waste circuit board, a solvent gasification low-temperature pyrolysis process is adopted, and due to the good in-situ hydrogen supply capacity of the solvent in the low-temperature pyrolysis process of the waste circuit board, halogen elements in a pyrolysis product are more easily converted into HX (X is a halogen element), so that the removal of the halogen elements is facilitated; moreover, due to the excellent hydrogen supply capability of the solvent, the generation of coke in the pyrolysis process of the waste circuit board can be inhibited, the heavy polymerization and polycondensation of depolymerization products are effectively inhibited, the pyrolysis liquid phase product is lightened, the yield of phenol monomers is improved, and the content of clean fuel gas in the gas phase product is increased; due to the good dissolving performance of the solvent and the pyrolysis liquid phase product of the waste circuit board, the viscosity of the pyrolysis liquid phase product is reduced, and the flowing performance is improved.
(3) The device and the method for the low-temperature pyrolysis of the waste circuit board through solvent gasification can effectively separate metal and nonmetal substances in the waste circuit board, have obvious effect on degrading organic components of the waste circuit board, can obviously reduce the content of pollutants in a pyrolysis product, improve the utilization rate of the pyrolysis product, and have good application prospect.
Drawings
FIG. 1 is a schematic view of the solvent gasification low-temperature pyrolysis device for waste circuit boards according to the present invention;
FIG. 2 is a schematic view showing the internal structure of a pyrolysis reactor according to the present invention;
FIG. 3 is a schematic view of the internal structure of the material reaction apparatus according to the present invention;
FIG. 4 is a schematic view showing the internal structure of a solvent vaporizing apparatus according to the present invention;
FIG. 5 is a schematic view of the solvent gasification pyrolysis principle of the present invention;
FIG. 6 is a composition diagram of a pyrolysis liquid phase product for three examples of the invention.
The reference numbers are as follows:
1-inert gas bottle, 2-gas flowmeter, 3-gas inlet pipe, 4-gas heat-insulating electric jacket, 5-pyrolysis reactor, 6-material reaction device, 7-solvent gasification device, 8-solvent pump, 9-condensation box, 10-solvent evaporation device, 11-oil tank, 12-condensation pipe, 13-solvent tank, 14-alkaline washing tank, 15-adsorption box and 16-gas collection device. 501-sealing screw, 502-furnace cover handle, 503-temperature thermocouple, 504-furnace cover, 505-sealing ring, 506-water cooling jacket, 507-furnace cover heat preservation layer, 508-air outlet pipe heat preservation electric jacket, 509-air outlet pipe, 510-air outlet pipe converter, 511-silicon carbide rod, 512-heat preservation layer, 513-furnace shell, 514-temperature controller, 515-2 temperature control thermocouple, 516-furnace body and 517-2 air inlet; 601-material rack handle, 602-fixed movable buckle, 603-object placing steel frame, 604-crucible; 701-gas inlet, 702-liquid inlet and 703-gas outlet.
Detailed description of the invention
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described below clearly and completely, and it is obvious that the described embodiments are a part of the embodiments of the present invention, not all of the embodiments of the present invention. All other embodiments obtained by those skilled in the art without any creative effort based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a solvent gasification pyrolysis device for a waste circuit board, which comprises a pyrolysis reactor 5 and a solvent gasification device 7, wherein the pyrolysis reactor 5 is sequentially communicated with a condensing box 9, an oil tank 11, a condensing pipe 12, a solvent tank 13, an alkaline washing tank 14, an adsorption tank 15 and a gas collection device 16; the solvent gasification device 7 is provided with an air inlet 701, an air outlet 703 and a liquid inlet 702; the air outlet 703 is connected with one end of the air inlet pipe 3; the other end of the gas inlet pipe 3 extends into the bottom of the pyrolysis reactor 5; the gas inlet 701 is communicated with an inert gas bottle 1 through a pipeline; the liquid inlet 702 is sequentially communicated with a solvent pump 8 and a solvent tank 13; and a material reaction device 6 is arranged in the pyrolysis reactor 5. A solvent pump 8 capable of adjusting the flow rate is arranged between the solvent gasification device 7 and the solvent tank 13. A gas heat-insulating electric jacket 4 is arranged on a gas inlet pipe 3 connected between the solvent gasification device 7 and the pyrolysis reactor 5.
The solvent evaporation device 10 is arranged outside the oil tank 11.
The alkali washing tank is a two-stage alkali washing tank.
The adsorption tank is an active carbon adsorption tank.
As shown in FIG. 2, the pyrolysis reactor 5 of the invention is provided with a furnace shell 513, an insulating layer 512, a furnace body 516, a No. 2 temperature control thermocouple 515 which sequentially penetrates through the furnace shell 513 and the insulating layer 512 and is abutted to the furnace body 516, wherein the furnace shell 513 and the insulating layer 512 are arranged outside and inside the pyrolysis reactor 5; a silicon carbide rod 511 is arranged between the furnace body 516 and the insulating layer 512;
the pyrolysis reactor 5 is also provided with a No. 2 gas inlet 517 and a gas outlet pipe 509; the gas inlet pipe 3 is communicated with the pyrolysis reactor 5 through a No. 2 gas inlet; the gas outlet pipe 509 is communicated with the furnace body 516 and sequentially penetrates through the insulating layer 512 and the furnace shell 513;
a T-shaped furnace cover 504 and a temperature control thermocouple 503 which penetrates through the central shaft of the T-shaped furnace cover 504 are arranged above the furnace body 516; a furnace cover handle 502 is arranged above the T-shaped furnace cover 504, and a sealing ring 505 fixedly connected with the T-shaped furnace cover 504, a water cooling sleeve 506 arranged between the T-shaped furnace cover 504 and the furnace shell 513 and a furnace cover insulating layer 507 connected with the furnace body 516 are sequentially arranged below the T-shaped furnace cover 504;
the pyrolysis reactor 5 is also provided with a temperature controller 514 connected with the silicon carbide rod 511, the temperature control thermocouple 503, the temperature measuring thermocouple 515 and the air outlet pipe heat-insulating electric jacket 508.
The outlet pipe 509 is inclined downward.
An air outlet pipe heat-insulating electric heating jacket 508 is arranged outside the air outlet pipe outside the heat-insulating layer; the outlet pipe port is provided with an outlet pipe converter 510.
As shown in fig. 3, a material reaction device 6 of the present invention includes a plurality of layers of storage steel frames 603, and the multi-level storage steel frames 603 are connected by a fixed movable buckle 602; a material rack handle 601 is arranged on the storage steel frame 603;
the storage steel frame 603 is provided with a detachable crucible 604.
The invention also provides a method for pyrolyzing the waste circuit board by using the equipment, which comprises the following steps:
(1) adding an FR-4 type waste circuit board into a pyrolysis reactor, wherein a binder is epoxy resin, sealing, checking the air tightness in the pyrolysis reactor, and introducing inert gas into a solvent gasification device and the pyrolysis reactor through a gas inlet pipe to enable the atmosphere in the solvent gasification device and the pyrolysis reactor to be an oxygen-free atmosphere;
(2) when the atmosphere in the solvent gasification apparatus and the pyrolysis reactor is an oxygen-free atmosphere, the gas flow meter is adjusted so that the flow rate of the inert gas is controlled at 100 mL/min. The solvents respectively adopt ethanol, n-propanol and n-butanol, and the temperature in the solvent gasification device is controlled at 100 ℃ (ethanol), 120 ℃ (n-propanol) and 140 ℃ (n-butanol) by adjusting the setting program of a temperature controller; the temperature of the gas heat-preservation electric jacket is consistent with that of the solvent gasification device, the temperature rise rate in the pyrolysis reactor is controlled to be 10-20 ℃/min, the pyrolysis final temperature is controlled to be 500 ℃, the heat preservation time is controlled to be 1h, the temperature of the gas outlet pipe heat-preservation electric jacket is controlled to be 300 ℃, and the temperature of the solvent evaporation device is controlled to be 100 ℃ (ethanol), 120 ℃ (n-propanol) and 140 ℃ (n-butanol).
(3) When the temperature thermocouple shows that the temperature in the pyrolysis reactor reaches 200 ℃, starting a solvent pump to extract the solvent in a solvent tank, controlling the flow rate of the solvent to be 100mL/min, gasifying the solvent into a gasifying agent through a solvent gasification device, mixing the gasifying agent with inert carrier gas, and introducing the gasifying agent to the bottom of the pyrolysis reactor through a gas inlet pipe;
(4) in the pyrolysis process, organic components of the waste circuit board react with a gasifying agent and are separated into a pyrolysis liquid phase product and a gas phase product through a multi-stage condensing box, the condensed pyrolysis liquid phase product is collected through an oil tank, the pyrolysis liquid phase product extracts redundant solvent through a solvent evaporation device, and the redundant solvent flows into a solvent tank to be recycled in the whole system; HBr and CO are removed from the pyrolysis gas-phase product through a two-stage alkaline washing tank and an active carbon adsorption box2And waiting for the waste gas, and then collecting and using the waste gas through a gas collecting device.
In the step (1), the inert gas introduced into the solvent gasification device and the pyrolysis reactor is nitrogen.
The mol ratio of the gasifying agent to the carrier gas is controlled to be 1: 1.
The waste wiring board solvent gasification pyrolysis liquid phase product composition is shown in fig. 6 and table 3.
Comparative example 1
By adopting the electronic waste pyrolysis furnace disclosed in application No. 201710192797.3, a pyrolysis liquid product is collected through an oil tank, a gas product is collected through an air bag, the used raw material is an FR-4 type waste circuit board, and the adhesive is brominated epoxy resin. Controlling the pyrolysis temperature to be 500 ℃, keeping the temperature for 1h, and using nitrogen as protective gas. The content of each product of conventional pyrolysis of waste circuit boards is shown in table 1:
table 1 content of conventional pyrolysis products of waste wiring boards
For the pyrolysis of the traditional waste circuit board, the pyrolysis product is divided into three parts, namely pyrolysis liquid phase, gas phase and solid phase products, bromine is mainly existed in the liquid phase and the gas phase, and the bromine is mainly existed in compounds such as 2-bromophenol, 2-bromo-4-isopropylphenol, 2, 6-dibromophenol and the like in the liquid phase product in the form of organic bromine; the gas phase product is present in HBr mainly as inorganic bromine. Analysis on the pyrolysis products of the traditional waste circuit boards shows that the pyrolysis liquid phase products have complex components, wide boiling range, poor flow property and high halogen content, and limit the use value of the pyrolysis liquid phase products.
Comparative example 2
The waste circuit board solvent gasification pyrolysis device of example 1 is adopted for gasification pyrolysis, deionized water is adopted as a solvent, the same raw material as that of comparative example 1, a waste circuit board of FR-4 model is used, and epoxy resin is used as a binder. Controlling the final temperature of pyrolysis to be 500 ℃, the heating rate to be 20 ℃/min, the heat preservation time to be 1h, the protection temperature of an air outlet pipe to be 300 ℃, the protection gas to be nitrogen, the flow rate of nitrogen to be 100mL/min, the evaporation temperature of the solvent to be 120 ℃ and the flow rate of the solvent to be 100 mL/min. The content of each product of steam pyrolysis of the waste circuit board is shown in table 2:
TABLE 2 waste wiring board steam pyrolysis product content
Compared with the traditional pyrolysis, the steam pyrolysis consumes carbon black in a pyrolysis solid-phase product through a water gas reaction, and obviously increases clean fuel gas (H) in a pyrolysis gas-phase product2CO, etc.), but the product quality of the pyrolysis liquid phase product is not changed, the organic bromine content of the pyrolysis liquid phase product is still high.
Three examples were described above: the conventional, steam and solvent gasification pyrolysis gas and solid phase products of the waste cord plate are compared as shown in table 3:
TABLE 3 comparison table of conventional, steam and solvent gasification pyrolysis gas phase and solid phase products of waste circuit board
Compared with the traditional pyrolysis and steam pyrolysis, the solvent gasification pyrolysis enables organic bromine to be converted into inorganic bromine through in-situ hydrogen supply capacity, the content of bromine-containing compounds is greatly reduced, and the content of phenolic compounds is greatly increased. Compared with the traditional pyrolysis, the content of bromine-containing compounds in the liquid-phase products of the gasification pyrolysis of the ethanol, the n-propanol and the n-butanol is respectively reduced by 93.53%, 94.09% and 94.66%, and the content of phenolic compounds is respectively improved by 44.59%, 46.36% and 47.00%; compared with steam pyrolysis, the content of bromine-containing compounds in the liquid-phase products of the gasification pyrolysis of the ethanol, the n-propanol and the n-butanol is respectively reduced by 93.30%, 93.89% and 94.47%, and the content of phenolic compounds is respectively improved by 51.68%, 53.22% and 53.77%. The solvent gasification pyrolysis is beneficial to improving the product quality of the pyrolysis liquid phase product, reducing the complexity of the product components, enhancing the product flow property, greatly reducing the halogen content and improving the use value.
The solvent gasification pyrolysis can provide hydrogen free radicals, effectively inhibits the heavy polymerization and polycondensation reaction of depolymerization products, reduces the generation of coke, and enables the separation of metals and non-metal substances in the waste circuit board to be easier.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (8)
1. A method for pyrolyzing a waste circuit board by using a solvent gasification pyrolysis device is characterized by comprising the following steps:
(1) adding the waste circuit board into the pyrolysis reactor (5), sealing the pyrolysis reactor (5), and introducing inert gas to enable the atmosphere in the solvent gasification device (7) and the pyrolysis reactor (5) to be oxygen-free atmosphere;
(2) controlling the flow of inert gas at 100-;
(3) when the target temperature in the pyrolysis reactor (5) reaches 200 ℃, starting a solvent pump (8) to extract the solvent in the solvent tank (13), controlling the flow rate of the solvent to be 100-; in the pyrolysis process, organic components of the waste circuit board react with a gasifying agent and are separated into a pyrolysis liquid phase product and a gas phase product through a multi-stage condensing box (9), the condensed pyrolysis liquid phase product is collected through an oil tank (11), the pyrolysis liquid phase product is extracted with redundant solvent through a solvent evaporation device (10), and the redundant solvent flows into a solvent tank (13) to be recycled in the whole system; the pyrolysis gas phase product is subjected to waste gas removal through an alkaline washing tank (14) and an adsorption box (15), and then is collected through a gas collecting device (16);
the solvent gasification pyrolysis device comprises a pyrolysis reactor (5) and a solvent gasification device (7), wherein the pyrolysis reactor (5) is sequentially communicated with a condensing box (9), an oil tank (11), a condensing pipe (12), a solvent tank (13), an alkali washing tank (14), an adsorption tank (15) and a gas collection device (16); the solvent gasification device (7) is provided with an air inlet (701), a liquid inlet (702) and an air outlet (703); the air outlet (703) is communicated with one end of the gas inlet pipe (3); the gas inlet pipe (3) is communicated with the pyrolysis reactor (5); the gas inlet (701) is communicated with the inert gas bottle (1) through a pipeline; the liquid inlet (702) is communicated with a solvent pump (8) and a solvent tank (13) in sequence;
a material reaction device (6) is arranged in the pyrolysis reactor (5);
a gas heat-insulating electric heating jacket (4) is arranged on a gas inlet pipe (3) connected between the solvent gasification device (7) and the pyrolysis reactor (5).
2. The method according to claim 1, characterized in that the pyrolysis reactor (5) is formed by an outer and an inner furnace shell (513), an insulation layer (512), a furnace body (516); the furnace shell (513) is provided with a No. 2 temperature control thermocouple (515) which sequentially penetrates through the furnace shell (513) and the heat insulation layer (512) and is abutted against the furnace body (516); a silicon carbide rod (511) is arranged between the furnace body (516) and the heat-insulating layer (512);
the pyrolysis reactor (5) is also provided with a No. 2 air inlet (517) and an air outlet pipe (509); the gas inlet pipe (3) is communicated with the pyrolysis reactor (5) through a No. 2 gas inlet (517); the gas outlet pipe (509) sequentially penetrates through the furnace shell (513), the heat insulation layer (512) and the furnace body (516) and is communicated with the hearth;
a T-shaped furnace cover (504) and a temperature thermocouple (503) penetrating through the central shaft of the T-shaped furnace cover (504) are arranged above the furnace body (516); a sealing ring (505) fixedly connected with the T-shaped furnace cover (504), a water cooling sleeve (506) arranged between the T-shaped furnace cover (504) and the furnace shell (513), and a furnace cover heat-insulating layer (507) connected with the furnace body (516) are sequentially arranged below the T-shaped furnace cover (504);
the pyrolysis reactor (5) is also provided with a temperature controller (514) connected with the silicon carbide rod (511), the temperature thermocouple (503), the No. 2 temperature control thermocouple (515) and the air outlet pipe heat-insulating electric jacket (508).
3. A method according to claim 2, wherein the outlet duct (509) is downwardly inclined.
4. The method according to claim 3, characterized in that an outlet pipe thermal insulation electric jacket (508) is arranged outside the outlet pipe (509) outside the thermal insulation layer, and an outlet pipe converter (510) is arranged at the port of the outlet pipe.
5. The method according to claim 1, wherein the material reaction device (6) comprises a plurality of layers of object placing steel frames (603) and fixed movable buckles (602), and the object placing steel frames (603) are connected through the fixed movable buckles (602); a material rack handle (601) is arranged on the storage steel frame (603);
the object placing steel frame (603) is provided with a detachable crucible (604).
6. A method according to claim 1, characterized in that a solvent evaporation device (10) is arranged outside the tank (11).
7. The method according to claim 1, characterized in that the temperature of the solvent vaporizing device (7), the gas insulated electric jacket (4) and the solvent evaporating device (10) is controlled to be uniform.
8. The method of claim 1, wherein the solvent is one or more of ethanol, n-propanol, isopropanol, n-butanol, isobutanol.
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