WO2017157180A1 - 一种裂解气循环加热与微波结合的轮胎橡胶裂解方法 - Google Patents

一种裂解气循环加热与微波结合的轮胎橡胶裂解方法 Download PDF

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Publication number
WO2017157180A1
WO2017157180A1 PCT/CN2017/075471 CN2017075471W WO2017157180A1 WO 2017157180 A1 WO2017157180 A1 WO 2017157180A1 CN 2017075471 W CN2017075471 W CN 2017075471W WO 2017157180 A1 WO2017157180 A1 WO 2017157180A1
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Prior art keywords
gas
cracking
oil
composite
tire rubber
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PCT/CN2017/075471
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English (en)
French (fr)
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周昆
康琪
姚波
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四川宏图普新微波科技有限公司
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Publication of WO2017157180A1 publication Critical patent/WO2017157180A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/10—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal from rubber or rubber waste
    • 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
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/07—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of solid raw materials consisting of synthetic polymeric materials, e.g. tyres
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock
    • Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics

Definitions

  • the invention relates to a treatment technology of waste tires, in particular to a tire rubber cracking method and a cracking system thereof, and belongs to the technical field of waste treatment and resource utilization.
  • the treatment of used tires mainly includes the following methods: landfill method, incineration method, regeneration and cracking method, etc.
  • the current cracking methods include thermal cracking, microwave cracking and some improved vacuum cracking.
  • the cracking of used tires is the last key step in the comprehensive utilization of waste tires and turning waste into treasure. For a long time, due to the great attention of all walks of life, many researchers have carried out a lot of research and experimental work. However, due to various reasons, an ideal scale, industrialization, environmental protection requirements, and economically viable production lines have not yet been formed.
  • Thermal cracking refers to cracking by heating in the presence of a catalyst, and the thermal cracking temperature is up to 750 ° C.
  • the tire thermal cracking process requires a large amount of heat energy.
  • Conventional incineration and pyrolysis are oxidation and high temperature processes, with slow heat transfer and poor uniformity. It takes a long time to complete the cracking and the cracking time is inefficient. At the same time, on the one hand, it is necessary to maintain the high temperature required for cracking, and on the other hand, it requires a long cracking time, resulting in high energy consumption for cracking, low efficiency of cracking energy, and secondary environmental pollution.
  • thermal cracking technology as a way to deal with the problem of waste tires, there are also complex defects, that is, most of the first to pull out the ring wire in the waste tire, and then cut the waste tire into a block, into the cracking furnace or cracking tower High temperature cracking, many processing steps, long production process and low overall efficiency.
  • the application publication number is CN104531198A
  • the name is a thermal cracking method for used tires
  • the whole waste tire and the catalyst pass 300 ° C in the preheating chamber.
  • the flowing nitrogen gas at -450 ° C is preheated and then enters the cracking chamber and is cracked under a flowing nitrogen atmosphere at 600 ° C to 1000 ° C.
  • the patented method is a method of heating waste tires by simply using high temperature gas: in fact, waste tire rubber is a bad heat conductor, and high temperature gas acts on the surface of the tire, and it takes a long time to maintain high temperature to transfer heat energy into the tire interior, and for a long time. Maintaining high temperature causes heat dissipation to be large, and energy is wasted; and as the surface of the tire is cracked, it becomes a loose carbon surface layer, and its thermal conductivity is further deteriorated.
  • Microwave cracking technology is a relatively new cracking technology developed in recent years. Usually, the chemical bond is broken by microwave energy in an inert nitrogen atmosphere, and the macromolecular chain of the polymer is opened, and then the liquid oil, gas and carbon black are separated. Its inert nitrogen environment avoids the oxidation of organic matter and prevents the production of toxic substances such as furan. This control of the cracking environment greatly improves the stability qualities of various recycled products, especially carbon black. Therefore, the advantage of thermal cracking of tire microwave cracking is very obvious.
  • the announcement number is CN103333709A
  • the name is the disc type microwave continuous cracking device and the method for cracking waste rubber
  • the fourth issue of 2005, "Application of Microwave Technology in Waste Treatment” page 33 discloses microwave treatment of used tires.
  • waste tires contain various materials such as rubber and metal, and microwaves are simply used for heating and energy coupling ratio.
  • the actual cracking microwave energy consumption is higher; in addition to the selective heating of the microwave, and the positive feedback effect, the waste tire part is firstly cracked by heating first, resulting in poor crack uniformity, and only the cracking time can be prolonged to ensure the cracking completely. Lead to more microwave energy wasted.
  • the invention aims to solve the problem that the tire rubber has high energy consumption, low cracking efficiency, low cracking efficiency, environmental protection requirements, low controllability of the cracking process, and a new cracking method for the tire rubber.
  • the speciality of waste tires, the gas obtained by cracking the tire rubber is treated and combined with microwave cracking, and recycled for the cracking of tire rubber.
  • the cracking method of the invention can be The quality of the cracking has been improved, and the cracking efficiency has been improved.
  • the controllability of the cracking process is improved, and the generation of harmful toxic gases is avoided.
  • the treated liquid oil, gas and carbon residue are used as fuel to heat the circulating gas, thereby improving the recycling rate of resources and reducing environmental pressure.
  • the present invention is achieved by the following techniques:
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; pretreatment is mainly to clean the tire rubber, remove impurities, crush and other treatment;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • the gas medium is heated to 350 ° C ⁇ 700 ° C by a gas heating device; usually, the entire cracking process is carried out under anaerobic conditions, so the gas medium is selected for the oxygen-free gas.
  • step C The gas medium heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking, and the tire rubber is continuously cracked under the above-mentioned joint action, and continuously converted to obtain a solid product and a mixed gaseous product;
  • step D The mixed gaseous product obtained in step D is subjected to oil and gas separation to remove pyrolysis oil; the pyrolysis oil is recycled;
  • the flow rate of the gas introduced into the gas heating device is the same as the flow rate of the gas introduced into the composite cracking chamber in step D.
  • the portion of the gas that exits the cracking system is recycled.
  • the cracking device Before the cracking device is turned on, it needs to be treated with oxygen.
  • the oxygen can be carried out by nitrogen, carbon dioxide, water vapor, inert gas, etc.
  • the gas medium In the initial cracking, the gas medium can be heated to 350-700 °C nitrogen, carbon dioxide, water vapor, inert gas.
  • One or more of the combinations are used as the gaseous medium for initial cracking; after one cycle of cracking, the gaseous medium is the gas obtained by the oil and gas separation in the step E.
  • the tire rubber is pre-heated before being cracked, and the pre-heating is preheating the tire rubber to 100 ° C to 400 ° C.
  • the preheating of the rubber tire to be cracked can improve the ability of the waste rubber tire to absorb microwaves and absorb the microwave uniformity, and make the microwave more used for cracking of the waste rubber tire.
  • Wheel The tire rubber is preheated to 100 ° C ⁇ 400 ° C, can be preheated by hot water, hot oil, steam, heating cycle exhaust gas, burned anoxic exhaust gas or heated inert gas.
  • the microwave used is an electromagnetic wave of 300 MHz to 300 GHz, and one or a combination of one or more of 915 MHz ⁇ 50 MHz, 2450 MHz ⁇ 50 MHz, and 5.8 GHz ⁇ 100 MHz may be further selected.
  • step D the solid product is discharged after anaerobic cooling, and is recycled; in step E, the oil and gas separation method includes one or more of condensation, adsorption, electrostatic degreasing, and spraying.
  • the combination causes the cracked oil in the mixed gaseous product to be separated. Condensation is to make the oil vapor into a liquid by cooling.
  • Adsorption can be carried out by adsorbing materials such as activated carbon and adsorbent (such as silica gel, alumina, molecular sieve), electrostatic oil removal, spraying can use spray water, oil and the like. Liquid, remove oil mist, oil vapor.
  • the heating of the gaseous medium comprises heating the mixed gaseous product with the mixed gaseous product of the step D through a heat exchange device, and the temperature of the mixed gaseous product is high, so that the gaseous medium can be heated by heat exchange, thereby Save energy.
  • one or more of the cracked oil, the gas discharged after the oil and gas separation, and the carbon residue in the solid product are heated as a fuel by using the oil and gas separation in the step E. To achieve the purpose of self-sufficiency in heat.
  • the present invention provides a tire rubber cracking system for use in the cracking method of claim 1, comprising a microwave generator, a composite cracking chamber connected to the microwave generator, and an oil and gas separation device, wherein the composite cracking chamber is opened a composite cracking chamber inlet port and a composite cracking chamber outlet port, wherein the oil and gas separation device is provided with an oil gas separation device inlet port and an oil and gas separation device outlet port, and further comprises a gas heating device, wherein the gas heating device is provided with gas heating a gas inlet of the gas heating device and a gas outlet of the gas heating device, wherein the gas outlet of the gas heating device is connected to the gas inlet of the composite cracking chamber, and the gas separation device is connected to the gas inlet device The mouth is connected to the gas outlet of the composite cracking chamber.
  • the working process is: feeding the raw material to be cracked into the composite cracking chamber, and then opening the gas heating device connected with the composite cracking chamber to heat the gas medium in the gas heating device; after heating, opening the gas outlet of the gas heating device and compound cracking The air inlet of the cavity, at this time, the heated gas medium continues to pass through
  • the combined cracking chamber and the microwave generator fed into the composite cracking chamber simultaneously act on the tire rubber for cracking to obtain a solid product and a mixed gaseous product; the mixed gaseous product continuously flows out from the outlet of the composite cracking chamber, and enters from the inlet of the oil separation device.
  • the oil and gas separation device performs oil and gas separation, and part of the separated gas is introduced into the gas heating device, heated, and then introduced into the composite cracking chamber for cracking, and sequentially circulated; the gas that does not pass into the composite cracking chamber passes through The gas splitting port on the oil and gas separation device, the gas separation device and the gas heating device is discharged from the cracking system.
  • a plurality of microwave generators can be coupled to the composite cracking chamber to facilitate the feeding of microwaves of one or more frequencies into the composite cracking chamber, as well as greater microwave power.
  • the mixed gas in the composite cracking chamber (the mixture of the gaseous product produced by the cracking and the gas medium) also continuously flows out from the gas outlet of the composite cracking chamber. , enter the next link.
  • the cracking system discharges the gas out of the cracking system, and the solid product discharge channel discharges the solid product out of the cracking system, and the devices are connected into a closed circulating circulation system, except that the gas phase product is not obtained at the beginning of cracking.
  • the gaseous medium is nitrogen, carbon dioxide, water vapor and inert gas. The gaseous medium in all subsequent cycles is obtained by separating the mixed gaseous products obtained by the cracking.
  • the cracking system further includes a raw material preheating device connected to the composite cracking chamber.
  • the composite cracking chamber is further provided with a solid product discharge passage.
  • the oil and gas separation device, the oil gas separation device and the gas heating device are connected with a gas distribution port, and the gas distribution port can be provided with a plurality of gas distribution ports.
  • the oil and gas separation device comprises a tubular heat exchange condenser, a shell and tube condenser, an adsorption degreaser, a spray condenser, a spray condenser, a column plate condenser, a tube plate condenser, and an electrostatic oil remover.
  • the raw material preheating device comprises one or a combination of one of a hot air heater, an infrared heater, a rotary heating cylinder, a heated fluidized bed, and a heating bath.
  • the present invention passes a gaseous medium heated to a temperature of 350 ° C to 700 ° C into a composite cracking chamber, and simultaneously acts on the tire rubber with the microwave to perform cracking.
  • a gaseous medium heated to a temperature of 350 ° C to 700 ° C into a composite cracking chamber, and simultaneously acts on the tire rubber with the microwave to perform cracking.
  • the same amount of tire is cracked.
  • the cracking time is reduced by more than 20%
  • the cracking energy consumption is reduced by more than 30%
  • the cracking efficiency is greatly improved, and the production cost is saved; Technical effect.
  • the invention continuously cracks into a gaseous medium having a temperature of 350 ° C to 700 ° C.
  • the gas medium in this temperature range is forcibly flowed between the raw materials and sufficiently exchanges heat with the same, not only providing cracking energy, but more importantly It is to improve the performance of rubber tires to absorb microwaves, and then combine this feature with microwaves to fully improve the energy utilization of cracking and reduce the cracking time; it also improves the controllability of the cracking process and facilitates the control of cracking raw materials.
  • the temperature is effective to control the ratio of the non-condensable gas to the cracked oil in the mixed gaseous product and the quality of the cracked oil.
  • the gaseous medium is nitrogen, carbon dioxide, water vapor, inert gas
  • the gas obtained by the method of the invention is recycled for cracking, which not only saves the cost of the gaseous medium, but also avoids
  • the use of nitrogen, carbon dioxide, water vapor, and inert gases causes environmental hazards and reduces environmental stress.
  • the method of the invention is suitable for large-scale applications and meets environmental requirements and is economically viable method routes.
  • the invention preheats the tire rubber to 100 ° C to 400 ° C before cracking, heats the tire rubber through the high temperature gas medium in the preheating and cracking system, improves the temperature of the tire rubber, thereby improving the microwave absorption capacity of the tire rubber and improving the uniformity. Sexuality can also partially provide cracking energy, which greatly improves microwave utilization efficiency and further reduces energy consumption and cracking time.
  • the method of the invention greatly reduces the microwave energy consumption and improves the cracking efficiency while ensuring complete cracking of the tire.
  • the present invention heats the mixed gaseous product at a high temperature with a gaseous medium to recover heat energy; and uses the carbon residue obtained by cracking the raw material, the gas discharged from the cracking system after separation by oil and gas, and the liquid oil as a fuel to be heated to achieve energy self-sufficiency.
  • the purpose is to save production costs.
  • the cracking system of the present invention adds a gas heating device to the prior art, and innovatively changes the connection relationship between the devices in the system to form a system for circulating the gas obtained by cracking itself for cracking.
  • the structure is simple and the operation is simple.
  • Figure 1 is a schematic structural view of a cracking system of the present invention
  • Figure 2 is a flow chart of the method of the present invention
  • 1 microwave generator 2 composite cracking chamber, 21 composite cracking chamber inlet, 22 composite cracking chamber outlet, 23 solid product discharge channel, 3 gas heating device, 31 gas heating device outlet, 32 gas heating device inlet 4 gas distribution ports, 5 gas drive devices, 6 oil and gas separation devices, 61 oil and gas separation device outlets, 62 oil and gas separation device inlets, and 7 raw material preheating devices.
  • the oxygen is isolated during the cracking process.
  • the gas is turned on, one or several kinds of nitrogen gas, carbon dioxide, water vapor, and inert gas are exhausted; the gases are replaced by the circulation of the gas medium. Drop it.
  • the microwave output power is 10 to 2000 kW.
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • step C The gas heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product;
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • step F Passing a portion of the gas obtained by the oil and gas separation in the step E to the gas heating device described in the step C to be heated to 350 ° C for the cycle cracking in the step D, and the remaining portion is discharged, and the gas is introduced into the gas heating device.
  • the flow rate of the gas in is the same as the flow rate of the gaseous medium introduced into the composite cracking chamber in step D.
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • the gas medium is an inert gas
  • step C The gas heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product;
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • the gas heating device uses a gas heating device to heat the gas medium to 450 ° C;
  • the gaseous medium is water vapor;
  • step D the gas heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product;
  • the cracking microwave frequency is 2450 MHz ⁇ 50 MHz;
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • the gas heating device uses a gas heating device to heat the gas medium to 600 ° C; the gaseous medium is nitrogen;
  • step C The gas heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product; the microwave frequency is 915 MHz ⁇ 50 MHz.
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • step F Passing a portion of the gas obtained by the oil and gas separation in the step E to the gas heating device described in the step C to be heated to 600 ° C for the cycle cracking in the step D, and the remaining portion is discharged, and the gas is introduced into the gas heating device.
  • the flow rate of the gas in is the same as the flow rate of the gaseous medium introduced into the composite cracking chamber in step D.
  • Embodiment 2 In order to better implement the present invention, the present embodiment is further improved on the basis of Embodiment 2. The difference between this embodiment and Embodiment 2 is:
  • the gaseous medium of this embodiment is a mixture of nitrogen, water vapor, and carbon dioxide.
  • the tire rubber is preheated and then sent to the composite cracking chamber for cracking.
  • the preheating is to preheat the tire rubber to 100 °C.
  • Preheating the rubber tire to be cracked to improve the waste rubber tire The ability to absorb microwaves and the uniformity of microwave absorption, and the use of microwaves for the cracking of used rubber tires.
  • Embodiment 2 In order to better implement the present invention, the present embodiment is further improved on the basis of Embodiment 2. The difference between this embodiment and Embodiment 2 is:
  • the tire rubber is preheated and then sent to a composite cracking chamber for cracking.
  • the preheating is to preheat the tire rubber to 250 °C.
  • Embodiment 2 In order to better implement the present invention, the present embodiment is further improved on the basis of Embodiment 2. The difference between this embodiment and Embodiment 2 is:
  • the tire rubber is preheated and then sent to the composite cracking chamber for cracking.
  • the preheating is to preheat the tire rubber to 400 °C.
  • This embodiment further provides a superior cracking system for cracking on the basis of Embodiment 1, as shown in FIG. 1, the cracking system includes a microwave generator 1, and a composite cracking connected with the microwave generator 1.
  • a cavity 2 an oil and gas separation device 6, a composite cracking chamber inlet 21 and a composite cracking chamber outlet 22 are opened, and the oil and gas separation device 6 is provided with an oil and gas separation device inlet 62 and oil and gas
  • the gas outlet 61 of the separating device is further characterized by further comprising a gas heating device 3, wherein the gas heating device 3 is provided with a gas heating device inlet 32 and a gas heating device outlet 31, and the gas heating device inlet 32
  • the gas heating device outlet port 31 is in communication with the oil and gas separation device outlet port 31, and the oil and gas separation device inlet port 62 is in communication with the composite cracking chamber outlet port 22.
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • the gaseous medium of this embodiment is carbon dioxide
  • step D the gas medium heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product;
  • the microwave frequency is 5.8 GHz ⁇ 100 MHz;
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • step F Passing a portion of the gas obtained by the oil and gas separation in the step E to the gas heating device described in the step C to be heated to 600 ° C for the cycle cracking in the step D, and the remaining portion is discharged, and the gas is introduced into the gas heating device.
  • the flow rate of the gas in is the same as the flow rate of the gaseous medium introduced into the composite cracking chamber in step D.
  • the tire rubber is preheated prior to cracking, and the preheating is to preheat the tire rubber by 250 °C.
  • the embodiment further includes a solid product treatment, wherein the solid product obtained by the cracking is discharged after anaerobic cooling, and the solid product after the cracking contains steel wire and a large amount of carbon residue, which can be recycled.
  • the oil and gas separation method is condensation, and the condensation is performed by cooling the oil vapor into a liquid to separate the cracked oil.
  • the heating is performed by heating the gas obtained by separating the oil and gas with the mixed gaseous product in the step D by heat exchange means or by using the pyrolysis oil in the step E, step D
  • One or more of the carbonaceous slag in the solid product is heated.
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • the gas medium is heated to 600 ° C by using a gas heating device; the gas medium is a gas obtained by separating the mixed gaseous products obtained by one cycle cracking according to the embodiment;
  • step C The gas heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product;
  • the microwave frequency is a combination of 915 MHz ⁇ 50 MHz and 5.8 GHz ⁇ 100 MHz;
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • step F Passing a portion of the gas obtained by the oil and gas separation in the step E to the gas heating device described in the step C to be heated to 600 ° C for the cycle cracking in the step D, and the remaining portion is discharged, and the gas is introduced into the gas heating device.
  • the flow rate of the gas in is the same as the flow rate of the gaseous medium introduced into the composite cracking chamber in step D.
  • the tire rubber is preheated prior to cracking, and the preheating is to preheat the tire rubber to 250 °C.
  • the oil and gas separation method is spray degreasing, and the spray can use a liquid such as water or oil to remove oil mist and oil vapor.
  • the heating comprises heating the gas obtained by separating the oil and gas with the mixed gaseous product in the step D by heat exchange means or using the pyrolysis oil in the step E, the step One or more of the carbonaceous slag in the solid product described in D is heated.
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • step C The gas heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product; the microwave frequency is 5.8 GHz ⁇ 100 MHz and A combination of 2450MHz ⁇ 50MHz.
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • step F Passing a portion of the gas obtained by the oil and gas separation in the step E to the gas heating device described in the step C to be heated to 550 ° C for the cycle cracking in the step D, and the remaining portion is discharged, and the gas is introduced into the gas heating device.
  • the flow rate of the gas in is the same as the flow rate of the gaseous medium introduced into the composite cracking chamber in step D.
  • the gaseous medium is a combination of carbon dioxide and a gas obtained by separating the oil and gas in step E.
  • the tire rubber is preheated before being cracked, and the preheating is to preheat the tire rubber to 300 °C.
  • the heating comprises heating the gas obtained by separating the oil and gas with the mixed gaseous product in the step D by heat exchange means or using the pyrolysis oil in the step E, the step One or more of the carbonaceous slag in the solid product described in D is heated.
  • the oil and gas separation method is condensation, and the condensation is to make the oil vapor into a liquid by cooling.
  • the cracking system includes a microwave generator 1, a composite cracking chamber connected to the microwave generator 1, and an oil and gas separation device 6.
  • the composite cracking chamber 2 is provided with a composite cracking chamber inlet 21 and a composite cracking chamber outlet 22, and the oil and gas separation device 6 is provided with an oil and gas separation device inlet 62 and an oil and gas separation device outlet 61.
  • the utility model further comprises a gas heating device 3, wherein the gas heating device 3 is provided with a gas heating device inlet 32 and a gas heating device outlet 31, and the gas heating device inlet 32 and the oil and gas separation device outlet 61
  • the gas heating device air outlet 31 is in communication with the composite cracking chamber inlet 21, and the oil and gas separation device inlet 62 is in communication with the composite cracking chamber outlet port 22.
  • the cracking system also includes a feed preheating device 7 that is coupled to the composite cracking chamber 2.
  • the composite cracking chamber 2 is further provided with a solid product discharge passage 23, and a gas split port 4 is disposed on the oil and gas separation device 6, and the connecting passage of the oil gas separation device 6 and the gas heating device 3.
  • the oil and gas separation device 6 uses a tubular heat exchange condenser.
  • the raw material preheating device 7 employs an infrared heater.
  • a tire rubber cracking method for cracking gas circulation heating combined with microwave comprising the following steps:
  • A tire rubber pretreatment; mainly to wash the tire rubber, and then broken into small pieces of about 25cm 2 ;
  • step B The tire rubber pretreated in step A is sent to the composite cracking chamber;
  • step C The gas heated in step C is continuously introduced into the composite cracking chamber and the microwave is simultaneously applied to the tire rubber for cracking to obtain a solid product and a mixed gaseous product; the microwave frequency is a combination of 2450 MHz ⁇ 50 MHz and 915 MHz ⁇ 50 MHz.
  • step E the mixed gaseous product obtained in step D is subjected to oil and gas separation to remove the cracked oil;
  • step F Passing a portion of the gas obtained by the oil and gas separation in the step E to the gas heating device described in the step C to be heated to 600 ° C for the cycle cracking in the step D, and the remaining portion is discharged, and the gas is introduced into the gas heating device.
  • the flow rate of the gas in is the same as the flow rate of the gaseous medium introduced into the composite cracking chamber in step D.
  • the tire rubber is preheated prior to cracking, and the preheating is to preheat the tire rubber to 200 °C.
  • the solid product treatment treatment method of this embodiment is the same as that of the eighth embodiment.
  • the oil and gas separation method is adsorption, and the adsorption oil mist can be adsorbed by activated carbon adsorption and adsorbent adsorption.
  • the raw material preheating device of the present embodiment is a rotary heating cylinder, and the oil and gas separation device is an adsorption oil remover.
  • the oil and gas separation side adopts a condensation mode
  • the oil and gas separation device is a shell and tube type condenser
  • the raw material preheating device is a rotary heating tube.
  • step C the gaseous medium is heated to 500 ° C;
  • step F the gas is heated to 500 ° C;
  • the raw material is preheated, the raw material is preheated to 350 ° C;
  • the present embodiment of the cleavage solid product treatment method is the same as in Example 8.
  • the oil and gas separation method of this embodiment can be carried out by spraying.
  • the material is preheated using a heated fluidized bed.
  • the oil and gas separation device may be a spray condenser or a spray condenser.
  • step C the gaseous medium is heated to 600 ° C;
  • step F the gas is heated to 600 ° C;
  • the raw material When the raw material is preheated, the raw material is preheated to 200 ° C;
  • the raw material preheating device is a heating bath.
  • the above table can effectively improve the cracking efficiency and significantly reduce the microwave energy consumption; relatively, the cracking process is greatly accelerated, the pyrolysis oil is reduced in the high temperature environment, and the cracking is greatly improved. Oil quality and yield.

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Abstract

一种轮胎橡胶裂解方法，所述方法包括下述步骤：A、轮胎橡胶预处理；B、将步骤A预处理好的轮胎橡胶送入复合裂解腔（2）；C、采用气体加热装置（3）将气体介质加热至350℃～700℃；D、将步骤C加热的气体持续地通入复合裂解腔（2）与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；E、将步骤D得到的混合气态产物进行油气分离除去裂解油；F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置（3）中加热至350℃～700℃用于步骤D循环裂解。采用上述方法能有效减少裂解能耗及裂解时间，节约成本。

Description

一种裂解气循环加热与微波结合的轮胎橡胶裂解方法 技术领域
本发明涉及一种废旧轮胎的处理技术，尤其涉及一种轮胎橡胶裂解方法及其裂解系统，属于废料处理与资源利用技术领域。
背景技术
随着人们生活水平逐步提高和物流业高速发展，我国的私有车保有量和货车数量逐年提高。车辆数量的增加带动了经济的发展，同时汽车轮胎的消耗和磨损也产生了很多的垃圾——废旧轮胎。废旧轮胎的处理现已成为废物处理的难题。目前，对废旧轮胎的处理，主要有以下几种方法：掩埋法、焚烧法、再生利用及裂解法等，目前裂解方法包括热裂解、微波裂解以及一些改进的真空裂解等。废旧轮胎的裂解是废轮胎综合利用，变废为宝的最后一道关键步骤。长期以来，受到社会各界极大的关注，很多研究人员为此进行了大量的研究和实验工作。但由于种种原因至今仍没有形成一条理想的规模化、工业化、且符合环保要求，并在经济上可行的生产线。
热裂解是指通过在催化剂存在下加热使之裂解，热裂解温度最高可达750℃，轮胎热裂解过程需要消耗大量的热能。传统的焚烧和热解是氧化和高温过程，传热慢，均匀性差，要使其完全裂解需要较长的时间、裂解时间效率较低。同时一方面要维持裂解所需高温，另一方面需要较长的裂解时间，导致裂解能耗较高、裂解能源效率较低，并伴随次生环境污染。此外，热裂解技术作为处理废轮胎问题的途径，还存在方法复杂的缺陷，即大多要先将废轮胎里的环状钢丝拉出，再将废轮胎切割成块，投入裂解炉或裂解塔中进行高温裂解，加工环节多，生产流程长，整体效率低。如申请公布号为CN104531198A，名称为一种废旧轮胎的热裂解方法，将废旧轮胎整体与催化剂在预加热仓中通过300℃ ～450℃的流动氮气预加热后进入裂解仓，在600℃～1000℃的流动氮气氛围下进行裂解。该专利方法是一个单纯使用高温气体加热废旧轮胎裂解的方法：实际上，废旧轮胎橡胶是不良热导体，高温气体作用于轮胎表面，需要长时间维持高温才能将热能传入轮胎内部，而长时间的维持高温使热耗散变大，能量浪费多；而且随着轮胎表面的裂解，变成疏松的炭表层，其导热性能进一步变差。
微波裂解技术是近年来发展起来的一项比较新的裂解技术。通常是在惰性氮气体环境中利用微波能将化学键断开，打开高分子聚合物大分子链，而后经分离得到液油、燃气及炭黑。其惰性氮气环境避免了有机物的氧化过程，阻止了如呋喃等有毒物质的产生。这种对裂解环境的控制大大改善了各种回收产品，特别是炭黑的稳定性品质。因此，轮胎微波裂解相比热裂解优势十分明显。如公告号为CN103333709A，名称为圆盘式微波连续裂解装置及裂解废旧橡胶的方法、2005年第四期，《微波技术在废物处理中的应用》，第33页公开了微波处理废旧轮胎。但时至今日仍鲜见以微波裂解技术建成的废物处理工厂实际投用，结合我们的研究认为：废轮胎含有橡胶以及金属等多种材料，将微波简单的用于对其加热，能量耦合率较低，实际裂解微波能耗较高；此外微波的选择性加热、以及正反馈效应，废轮胎部分被先加热先裂解，导致裂解均匀性变差，为保证裂解完全只能延长裂解时间，从而导致更多的微波能浪费。
发明内容
本发明旨在解决轮胎橡胶在裂解过程中存在的耗能高，裂解效率低，裂解产物不符合环保要求，裂解处理过程可控性低等问题，提供一种新的轮胎橡胶的裂解方法，针对废旧轮胎的特殊性，将轮胎橡胶裂解得到的气体经过处理后与微波裂解进行创新性的结合，并循环用于轮胎橡胶的裂解，通过采用特定的方法步骤和参数，使得发明的裂解方法在能耗上有了质的降低，裂解效率有了质的提高，同时还提高了裂解处理过程的可控性，避免有害有毒气体的产生， 并将处理后的液油、气体、炭渣作为燃料，用于加热循环气体，提高资源的回收利用率，减轻环境压力。
为了解决上述技术问题，本发明通过以下技术实现：
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；预处理主要是将轮胎橡胶清洗、除杂、破碎等处理；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至350℃～700℃；通常，整个裂解过程都都是在无氧条件下进行，所以气体介质因选择无氧气体。
D、将步骤C加热的气体介质持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，轮胎橡胶在上述共同作用下持续的裂解，持续转化得到固态产物和混合气态产物；
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；裂解油回收利用；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至350℃～700℃用于步骤D循环裂解，其余部分排出裂解系统，不再参与循环，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体的流量相同。排出裂解系统的那一部分气体回收利用。
裂解装置开机前，需进行排氧处理，排氧可以氮气、二氧化碳、水蒸气、惰性气体等进行，初始裂解时，气体介质可以采用加热到350～700℃的氮气、二氧化碳、水蒸气、惰性气体中的一种或一种以上的组合作为初始裂解的气体介质；在裂解经过一个循环后，所述的气体介质为步骤E中经油气分离得到的气体。
进一步的，所述的轮胎橡胶裂解前进行预加热，所述预加热是将轮胎橡预加热至100℃～400℃。对要裂解的橡胶轮胎预加热可提高废旧橡胶轮胎吸收微波的能力和吸收微波的均匀性，并使微波更多的用于废旧橡胶轮胎裂解。将轮 胎橡胶预加热至100℃～400℃，可以采用热水、热油、蒸汽、加热循环尾气、燃烧后的缺氧尾气或者加热的惰性气体进行预加热。
在裂解时，使用的微波是一种300MHz～300GHz的电磁波，可进一步的选择频率为915MHz±50MHz、2450MHz±50MHz，5.8GHz±100MHz中的一种或一种以上的组合。
在步骤D中，所述固态产物经无氧冷却后排出，回收利用；在步骤E中，所述的油气分离方法包括冷凝、吸附、静电除油及喷淋中的一种或一种以上的组合使混合气态产物中的裂解油被分离出来。冷凝是用冷却的方法使油蒸汽变成液体，吸附可用活性碳、吸附剂(如硅胶、氧化铝、分子筛)等吸附材料吸附油雾，静电除油，喷淋可以采用喷洒水、油之类的液体，去除油雾、油蒸汽。
在步骤F中，所述气体介质加热包括将气体介质与步骤D所述混合气态产物通过换热装置换热进行加热，混合气态产物温度高，因此可通过换热的方式对气体介质加热，从而节约了能源。或利用步骤E中油气分离得到裂解油、油气分离后被排出的气体、所述固态产物中的炭渣中的一种或多种作为燃料进行加热。达到热量自给自足的目的。
进一步的，本发明还提供了一种用于权利要求1裂解方法的轮胎橡胶裂解系统，包括微波发生器、与微波发生器连接的复合裂解腔、油气分离装置，所述复合裂解腔上开设有复合裂解腔进气口和复合裂解腔出气口，所述油气分离装置上开设有油气分离装置进气口和油气分离装置出气口，还包括气体加热装置，所述气体加热装置上开设有气体加热装置进气口和气体加热装置出气口，所述气体加热装置进气口与油气分离装置出气口连通，所述气体加热装置出气口与复合裂解腔进气口连通，所述油气分离装置进气口与复合裂解腔出气口连通。其工作流程为：将需裂解的原料送入复合裂解腔，然后开启与复合裂解腔连接的气体加热装置将气体加热装置中的气体介质加热；加热好后打开气体加热装置的出气口、复合裂解腔的进气口，此时加热好的气体介质持续地通入复 合裂解腔与微波发生器馈入复合裂解腔的微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；混合气态产物从复合裂解腔出气口持续流出，从油气分离装置进气口进入油气分离装置进行油气分离，分离得到的气体中的部分通入到气体加热装置中加热后再通入到复合裂解腔中用于裂解，依次循环；没有通入到复合裂解腔中的气体则通过油气分离装置上、油气分离装置与气体加热装置的连接通道上的气体分流口排出裂解系统。
进一步的，可在复合裂解腔上连接多个微波发生器，以便于能向复合裂解腔中馈入一种或多种频率的微波，以及更大的微波功率。
在向复合裂解腔持续的通入气体介质的裂解的过程中，复合裂解腔中的混合气体(为裂解产生的气态产物和通入气体介质的混合)也同时持续地从复合裂解腔出气口流出，进入下一环节。
本裂解系统除了气体分流口将气体排出裂解系统外、固态产物排出通道将固态产物排出裂解系统外，各装置之间连接成一个循环流通的密闭系统，除了刚开始裂解，没有得到混合气态产物的情况下气体介质为氮气、二氧化碳、水蒸气和惰性气体，后面所有的循环过程中的气体介质都是将裂解得到的混合气态产物经油气分离得到的。
进一步的，所述裂解系统还包括原料预加热装置，所述原料预加热装置与复合裂解腔连接。
所述复合裂解腔上还设有固体产物排出通道，所述油气分离装置上、油气分离装置与气体加热装置的连接通道上设有气体分流口，气体分流口可设置多个。
所述油气分离装置包括管式换热冷凝器、壳管式冷凝器、吸附除油器、喷雾式冷凝器、喷淋式冷凝器、列板式冷凝器、管板式冷凝器、静电除油器中的任意一种或一种以上的组合，所述原料预加热装置包括热风式加热器、红外加热器、回转加热筒、加热流化床、加热浴槽中的一种或一种以上的组合。
本发明的有益效果：
1、本发明将加热至350℃～700℃的气体介质通入复合裂解腔，与微波同时作用于轮胎橡胶从而进行裂解，通过这一特定的方法步骤和参数的结合，在裂解同样量的轮胎橡胶时，与传统的热裂解方法、微波裂解方法相比，裂解时间减少了20％以上，裂解能耗降低了30％以上，大大的提高了裂解效率，节省了生产成本；取得了意料不到的技术效果。本发明持续地的通入温度为350℃～700℃的气体介质进行裂解，这一温度范围的气体介质强制性的从原料之间流过并与之充分换热，不仅提供裂解能量，更重要的是改善橡胶轮胎吸收微波的性能，再将这一特点与微波特定地结合，从而充分提高裂解的能源利用率，减少了裂解时间；还提高了裂解进程的可控性，便于控制裂解原料的温度，从而有效控制混合气态产物中不凝性气体与裂解油的比例、裂解油的品质。
本发明在初始裂解的时候的气体介质为氮气、二氧化碳、水蒸气、惰性气体这些气体，后续都将按本发明方法得到的气体循环用于裂解，不但节省了气体介质的成本，同时还能避免了使用氮气、二氧化碳、水蒸气、惰性气体这些气体造成环境危害问题，减轻了环境压力。
本发明方法适合大规模应用，且符合环保要求，并在经济上可行的方法路线。
2、本发明在裂解前将轮胎橡胶预加热至100℃～400℃，通过预热和裂解系统中的高温气体介质加热轮胎橡胶，提高轮胎橡胶温度，从而改善轮胎橡胶的微波吸收能力、提高均匀性，还能部分地提供裂解能量，从而极大地提高微波利用效率，进一步减少能耗及裂解时间。
3、采用本发明的方法，在保证轮胎的完全裂解的同时，极大的降低了微波能耗，并提高了裂解效率。
4、本发明将高温的混合气态产物与气体介质换热，从而回收热能；并利用原料裂解后得到的炭渣、经油气分离后排出裂解系统的气体、液油作为燃料进行加热，达到能量自足的目的，节省生产成本。
5、本发明的裂解系统在现有技术的基础上增加了气体加热装置，并创新性的改变系统中各装置之间的连接关系，形成一个可以将裂解自身得到的气体循环用于裂解的系统，结构简单，操作简单。
附图说明
图1为本发明裂解系统结构示意图；
图2为本发明方法流程图；
1微波发生器、2复合裂解腔、21复合裂解腔进气口、22复合裂解腔出气口、23固态产物排出通道、3气体加热装置、31气体加热装置出气口、32气体加热装置进气口、4气体分流口、5气体驱动装置、6油气分离装置、61油气分离装置出气口、62油气分离装置进气口、7原料预加热装置。
具体实施方式
下述实施例中，裂解过程中是隔绝氧气的，每次开机需通入氮气、二氧化碳、水蒸气、惰性气体的一种或几种排出系统内空气；这些气体随着气体介质的循环被替换掉。
下述实施例中，微波输出功率为10～2000kw。
实施例1
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至350℃；
D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至350℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
实施例2
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至700℃；气体介质为惰性气体；
D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至700℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
实施例3
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至450℃；气体介质为水蒸气；
D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；裂解的微波频率为2450MHz±50MHz；
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至450℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
实施例4
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至600℃；气体介质为氮气；
D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；微波频率为915MHz±50MHz。
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至600℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
实施例5
为了更好的实施本发明，本实施例在实施例2的基础上进一步改进，本实施例与实施例2的区别在于：
本实施例的气体介质为氮气、水蒸气、二氧化碳的混合。
本实施例将轮胎橡胶进行预加热后再送入复合裂解腔进行裂解，所述预加热是将轮胎橡预加热至100℃。对要裂解的橡胶轮胎预加热可提高废旧橡胶轮胎 吸收微波的能力和吸收微波的均匀性，并使微波更多的用于废旧橡胶轮胎裂解。
实施例6
为了更好的实施本发明，本实施例在实施例2的基础上进一步改进，本实施例与实施例2的区别在于：
本实施例将轮胎橡胶进行预加热后再送入复合裂解腔进行裂解，所述预加热是将轮胎橡预加热至250℃。
实施例7
为了更好的实施本发明，本实施例在实施例2的基础上进一步改进，本实施例与实施例2的区别在于：
本实施例将轮胎橡胶进行预加热后再送入复合裂解腔进行裂解，所述预加热是将轮胎橡预加热至400℃。
实施例8
本实施例在实施例1的基础上，进一步提供了较优的用于裂解的裂解系统，如图1所示，所述的裂解系统包括微波发生器1、与微波发生器1连接的复合裂解腔2、油气分离装置6，所述复合裂解腔2上开设有复合裂解腔进气口21和复合裂解腔出气口22，所述油气分离装置6上开设有油气分离装置进气口62和油气分离装置出气口61，其特征在于：还包括气体加热装置3，所述气体加热装置3上开设有气体加热装置进气口32和气体加热装置出气口31，所述气体加热装置进气口32与油气分离装置出气口61连通，所述气体加热装置出气口31与复合裂解腔进气口21连通，所述油气分离装置进气口62与复合裂解腔出气口22连通。
实施例9
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至600℃；本实施例的气体介质为二氧化碳；
D、将步骤C加热的气体介质持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；微波频率为5.8GHz±100MHz；
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至600℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
所述的轮胎橡胶裂解前进行预加热，所述预加热是将轮胎橡预加热250℃。
本实施例还包括固态产物处理，所述固态产物处理是将裂解得到的固态产物经无氧冷却后排出、裂解后的固态产物中含有钢丝和大量的炭渣，可回收利用。
本实施例中，所述的油气分离方法为冷凝，冷凝是用冷却的方法使油蒸汽变成液体从而将裂解油分离出来。
本实施例中的步骤F中，所述加热是将油气分离得到的气体与步骤D中所述混合气态产物通过换热装置换热的方式进行加热或利用步骤E中所述裂解油、步骤D中所述固态产物中的炭渣中的一种或多种燃料进行加热。
实施例10
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至600℃；气体介质为按本实施例经过一个循环裂解得到的混合气态产物经油气分离处理后得到的气体；
D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；微波频率为915MHz±50MHz和5.8GHz±100MHz的组合；
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至600℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
本实施例中，所述的轮胎橡胶裂解前进行预加热，所述预加热是将轮胎橡预加热至250℃。
本实施例中，所述的油气分离方法为喷淋除油，喷淋可以采用喷洒水、油之类的液体，去除油雾、油蒸汽。
本实施例中，在步骤F中，所述加热包括将油气分离得到的气体与步骤D中所述混合气态产物通过换热装置换热的方式进行加热或利用步骤E中所述裂解油、步骤D中所述固态产物中的炭渣中的一种或多种燃料进行加热。
实施例11
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，所述方法包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至550℃；
D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；微波频率为5.8GHz±100MHz和 2450MHz±50MHz的组合。
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至550℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
本实施例中，气体介质为二氧化碳与步骤E油气分离得到的气体的组合。
进一步的，所述的轮胎橡胶裂解前进行预加热，所述预加热是将轮胎橡预加热至300℃。
本实施例中，在步骤F中，所述加热包括将油气分离得到的气体与步骤D中所述混合气态产物通过换热装置换热的方式进行加热或利用步骤E中所述裂解油、步骤D中所述固态产物中的炭渣中的一种或多种燃料进行加热。
所述的油气分离方法为冷凝，冷凝是用冷却的方法使油蒸汽变成液体。
本实施例提供了另一种用于本发明的较佳的裂解系统，如图1所示，该裂解系统包括微波发生器1、与微波发生器1连接的复合裂解腔2、油气分离装置6，所述复合裂解腔2上开设有复合裂解腔进气口21和复合裂解腔出气口22，所述油气分离装置6上开设有油气分离装置进气口62和油气分离装置出气口61，其特征在于：还包括气体加热装置3，所述气体加热装置3上开设有气体加热装置进气口32和气体加热装置出气口31，所述气体加热装置进气口32与油气分离装置出气口61连通，所述气体加热装置出气口31与复合裂解腔进气口21连通，所述油气分离装置进气口62与复合裂解腔出气口22连通。所述裂解系统还包括原料预加热装置7，所述原料预加热装置7与复合裂解腔2连接。所述复合裂解腔2上还设有固体产物排出通道23，所述油气分离装置6上、油气分离装置6与气体加热装置3的连接通道上设有气体分流口4。
所述油气分离装置6采用的是管式换热冷凝器。
所述原料预加热装置7采用的是红外加热器。
实施例12
一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，包括下述步骤：
A、轮胎橡胶预处理；主要是将轮胎橡胶进行清洗，然后破碎成25cm2左右的小块；
B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
C、采用气体加热装置将气体介质加热至650℃；
D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；微波频率为2450MHz±50MHz和915MHz±50MHz的组合。
E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至600℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
所述的轮胎橡胶裂解前进行预加热，所述预加热是将轮胎橡预加热至200℃。
本实施例固态产物处理处理方式与实施例8相同。
所述的油气分离方法为吸附，可采用活性炭吸附以及吸附剂吸附等吸附油雾。
本实施例与实施例11中的裂解系统的区别在于：
本实施的原料预加热装置为回转加热筒，所述油气分离装置为吸附除油器。
实施例13
本实施例与实施例11的区别在于：本实施例中，油气分离方采用冷凝方式，所述油气分离装置为壳管式冷凝器，原料预加热装置为回转加热筒。
实施例14
本实施例与实施例11的区别在于：
步骤C中，气体介质加热至500℃；
步骤F中，气体加热至500℃；
进行原料预加热时，原料预加热至350℃；
本实施裂解固态产物处理方法实施例8相同。
本实施例的油气分离方法可采用喷淋进行。
原料预加热采用加热流化床。
所述油气分离装置可采用喷雾式冷凝器或是喷淋式冷凝器。
实施例15
本实施例与实施例14的区别在于：
步骤C中，气体介质加热至600℃；
步骤F中，气体加热至600℃；
进行原料预加热时，原料预加热至200℃；
本实施例中，原料预加热装置为加热浴槽。
将实施例1-14的相关数据统计在下表1中；
表1
Figure PCTCN2017075471-appb-000001
Figure PCTCN2017075471-appb-000002
由上述1数据可知：由上述表格数据可知：本方法有效提高裂解效率并显著降低微波能耗；相对的，大幅的加速了裂解过程，减少裂解油在高温环境的时间，极大的提高了裂解油的品质和产量。
以上所述，仅是本发明的较佳实施例，并非对本发明做任何形式上的限制，凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化，均落入本发明的保护范围之内。

Claims (10)

  1. 一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，其特征在于：所述方法包括下述步骤：
    A、轮胎橡胶预处理；
    B、将步骤A预处理好的轮胎橡胶送入复合裂解腔；
    C、采用气体加热装置将气体介质加热至350℃～700℃；
    D、将步骤C加热的气体持续地通入复合裂解腔与微波同时作用于轮胎橡胶进行裂解，得到固态产物和混合气态产物；
    E、将步骤D得到的混合气态产物进行油气分离除去裂解油；
    F、将步骤E中经油气分离得到的气体中的部分通入到步骤C所述的气体加热装置中加热至350℃～700℃用于步骤D循环裂解，其余部分排出，所述通入到气体加热装置中的气体的流量与步骤D中通入到复合裂解腔中的气体介质的流量相同。
  2. 根据权利要求1所述的一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，其特征在于：步骤C中所述气体介质包括氮气、二氧化碳、水蒸气、惰性气体和所述步骤E中经油气分离得到的气体的一种或一种以上的组合。
  3. 根据权利要求1所述的一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，其特征在于：所述的轮胎橡胶裂解前进行预加热，所述预加热是将轮胎橡预加热至100℃～400℃。
  4. 根据权利要求1所述的一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，其特征在于：所述裂解的微波频率包括915MHz±50MHz、2450MHz±50MHz，5.8GHz±100MHz中的一种或一种以上的组合。
  5. 根据权利要求1所述的一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，其特征在于：在步骤D中，所述固态产物经无氧冷却后排出，回收利用；在步骤E中，所述的油气分离方法包括冷凝、吸附、静电及喷淋中的一种或一种以上的组合。
  6. 根据权利要求5所述的一种裂解气循环加热与微波结合的轮胎橡胶裂解方法，其特征在于，在步骤F中，所述加热包括将油气分离得到的气体与步骤D中所述混合气态产物通过换热装置换热的方式进行加热；或利用步骤E中油气分离得到的气体和裂解油、步骤D中所述固态产物中的炭渣中的一种或多种作为燃料进行加热。
  7. 一种用于权利要求1橡胶裂解方法的轮胎橡胶裂解系统，包括微波发生器(1)、与微波发生器(1)连接的复合裂解腔(2)、油气分离装置(6)，所述复合裂解腔(2)上开设有复合裂解腔进气口(21)和复合裂解腔出气口(22)，所述油气分离装置(6)上开设有油气分离装置进气口(62)和油气分离装置出气口(61)，其特征在于：还包括气体加热装置(3)，所述气体加热装置(3)上开设有气体加热装置进气口(32)和气体加热装置出气口(31)，所述气体加热装置进气口(32)与油气分离装置出气口(61)连通，所述气体加热装置出气口(31)与复合裂解腔进气口(21)连通，所述油气分离装置进气口(62)与复合裂解腔出气口(22)连通。
  8. 根据权利要求7所述的裂解系统，其特征在于：所述裂解系统还包括原料预加热装置(7)，所述原料预加热装置(7)与复合裂解腔(2)连接。
  9. 根据权利要求7所述的裂解系统，其特征在于：所述复合裂解腔(2)上还设有固体产物排出通道(23)，所述油气分离装置(6)上、油气分离装置(6)与气体加热装置(3)的连接通道上设有气体分流口(4)。
  10. 根据权利要求8所述的裂解系统，其特征在于：所述油气分离装置(6)包括管式换热冷凝器、壳管式冷凝器、吸附除油器、喷雾式冷凝器、喷淋式冷凝器，列板式冷凝器、管板式冷凝器、静电除油器中的任意一种或一种以上的组合，所述原料预加热装置(7)包括热风式加热器、红外加热器、回转加热筒、加热流化床、加热浴槽中的一种或一种以上的组合。
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