WO2024234459A1 - 一种两阶段共液化混合-反应-过滤-热回收一体式装置 - Google Patents

一种两阶段共液化混合-反应-过滤-热回收一体式装置 Download PDF

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Publication number
WO2024234459A1
WO2024234459A1 PCT/CN2023/105230 CN2023105230W WO2024234459A1 WO 2024234459 A1 WO2024234459 A1 WO 2024234459A1 CN 2023105230 W CN2023105230 W CN 2023105230W WO 2024234459 A1 WO2024234459 A1 WO 2024234459A1
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Prior art keywords
stage
liquefaction
hydrothermal liquefaction
hydrothermal
reaction
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English (en)
French (fr)
Inventor
徐东海
郝博天
刁云飞
魏涯
徐铭欣
郭洋
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Xian Jiaotong University
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Xian Jiaotong University
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Priority to US18/746,484 priority Critical patent/US20240383791A1/en
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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
    • C10G1/02—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
    • 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
    • C10G1/008—Controlling or regulating of liquefaction processes
    • 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
    • C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts

Definitions

  • the invention relates to the technical field of hydrothermal liquefaction equipment, and in particular to a two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device.
  • Co-hydrothermal liquefaction is a method of combining two or more raw materials for hydrothermal liquefaction. Mixing different materials together to participate in the reaction can not only produce a simple superposition effect, but also produce a composite effect due to the synergistic or antagonistic effects of these materials. Experimental studies have found that co-hydrothermal liquefaction between different material compositions has a significant synergistic effect, and high-quality and high-yield bio-crude oil can often be obtained. Therefore, the development of advanced and efficient co-hydrothermal liquefaction technology, efficient biomass conversion, and biomass resource utilization have become a new direction for the development of hydrothermal technology.
  • Two-stage hydrothermal liquefaction is a hydrothermal treatment at low temperature in the first stage, followed by hydrothermal liquefaction under more stringent conditions.
  • the presence of low-temperature hydrothermal treatment significantly affects the final elemental composition, HHV, energy recovery rate, molecular components, TOC concentration of the aqueous phase, and solid yield.
  • the potential energy consumption savings and reduced reaction temperature lead to reduced equipment costs, which shows that two-stage hydrothermal liquefaction is an ideal liquefaction process.
  • the traditional hydrothermal liquefaction reactor is a simple tubular reactor.
  • the purpose of the present invention is to provide a two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device to solve the technical problems in the prior art that the mixing efficiency of various materials and media is low; the material mixer, reactor, solid phase product filter, and heat recovery of the hydrothermal liquefaction are separate and complex in structure, and two-stage hydrothermal liquefaction cannot be achieved; and the biomass has the problem of excessively high temperature and salt deposition that seriously blocks the pipeline.
  • a two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device comprises a first-stage hydrothermal liquefaction generating chamber, a second-stage hydrothermal liquefaction generating chamber and a medium-temperature hydrothermal transition product collection box; a plurality of material feed ports and a medium feed port are arranged on one side of the top of the first-stage hydrothermal liquefaction generating chamber, a high-temperature hydrothermal product feed port is arranged on the other side of the top, a hydrothermal final product discharge port is arranged on the bottom, a plurality of first-stage hydrothermal liquefaction reaction tubes are arranged longitudinally inside, the plurality of first-stage hydrothermal liquefaction reaction tubes are connected in sequence, one end of each first-stage hydrothermal liquefaction reaction tube extends out through the inner wall of the first-stage hydrothermal liquefaction generating chamber and is connected to the input end of the medium-temperature hydrothermal transition product collection box, and one end of
  • a nozzle is provided between the plurality of material feed ports and the medium feed port and one end of the first-stage hydrothermal liquefaction reaction tube at the top, wherein one end of the nozzle is provided with multiple pipelines, which are sequentially connected to the plurality of material feed ports and the medium feed port, and the other end of the nozzle is a single pipeline, which is connected to one end of the first-stage hydrothermal liquefaction reaction tube;
  • a receiving tube, a mixing tube and a diffusion tube are arranged in sequence between the single pipeline and one end of the first-stage hydrothermal liquefaction reaction tube, wherein the receiving tube, the mixing tube and the diffusion tube are all of different diameter structures.
  • each first-stage hydrothermal liquefaction reaction tube is provided with an inclination angle of 1-3°.
  • a high-temperature and high-pressure needle valve is provided at one end of each first-stage hydrothermal liquefaction reaction tube close to the medium-temperature hydrothermal transition product manifold and between each first-stage hydrothermal liquefaction reaction tube.
  • an electric heating coil is provided between the second insulation layer and the outer wall of the second-stage hydrothermal liquefaction chamber.
  • a filter screen is provided on the top of the first baffle cylinder, and the slag cleaning mechanism extends into the first baffle cylinder through the filter screen.
  • the slag cleaning mechanism includes a motor, a rotating shaft, a slag scraping device and a salt scraping device; one end of the rotating shaft is equipped with the motor, and the other end extends into the first baffle cylinder through a filter screen, and the slag scraping device and the salt scraping device are respectively installed on the rotating shaft in the first baffle cylinder.
  • a microwave controller is provided on the first-stage hydrothermal liquefaction chamber, and a plurality of microwave generators are provided on both the first-stage hydrothermal liquefaction chamber and the second-stage hydrothermal liquefaction chamber.
  • the present invention has the following beneficial technical effects:
  • the present invention provides a two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device, which realizes the two-stage hydrothermal liquefaction process; secondly, nozzles, receiving chambers, mixing chambers and diffusion chambers are arranged at the inlets of different materials and media, and high-speed fluids are collided and mixed in these structures; thirdly, the heat of hydrothermal liquefaction in the first stage comes from the heat of the hydrothermal liquefaction product in the second stage, and at the same time, the occurrence of the hydrothermal liquefaction reaction in the first stage and the recovery rate of the heat of the hydrothermal liquefaction product in the second stage are realized, thereby improving the efficiency of the hydrothermal liquefaction process.
  • the economic efficiency is improved; secondly, in the first stage of hydrothermal liquefaction, the high temperature and high pressure needle valve is set to achieve precise control of different reaction times, so that different first stage hydrothermal liquefaction reaction times can be selected according to different material characteristics; finally, the first stage hydrothermal liquefaction reaction tube is set with a 1-3° inclination, and the second stage hydrothermal liquefaction chamber is equipped with a scraper device and a salt scraper device to ensure the stable operation of the reactor.
  • the device is a highly integrated device that realizes the coupling of mixing, reaction, filtration, and heat recovery processes, greatly reducing the complexity and construction cost of the system, and utilizing the new liquefaction process of co-hydrothermal liquefaction and two-stage hydrothermal liquefaction to obtain high-yield and high-quality bio-crude oil, improve the economy of the system, and promote the industrialization development of hydrothermal liquefaction technology.
  • a nozzle is provided between the plurality of material feed ports and the medium feed port and one end of the first-stage hydrothermal liquefaction reaction tube at the top, wherein one end of the nozzle is provided with multiple pipelines, which are sequentially connected to the plurality of material feed ports and the medium feed port, and the other end of the nozzle is a single pipeline, which is connected to one end of the first-stage hydrothermal liquefaction reaction tube, and a receiving tube, a mixing tube and a diffusion tube are sequentially provided between the single pipeline and one end of the first-stage hydrothermal liquefaction reaction tube, wherein the receiving tube, the mixing tube and the diffusion tube are all of different diameter structures, thereby improving the mixing efficiency between the plurality of materials and the medium.
  • a high-temperature and high-pressure needle valve is provided at one end of each first-stage hydrothermal liquefaction reaction tube close to the medium-temperature hydrothermal transition product collection box and between each first-stage hydrothermal liquefaction reaction tube.
  • the outflow of the first-stage hydrothermal liquefaction product is controlled by opening and closing the high-temperature and high-pressure needle valve, thereby achieving precise control of the first-stage hydrothermal liquefaction reaction time.
  • a plurality of catalyst grids are provided in the catalytic zone between the second baffle tube and the first baffle tube, which effectively promote the occurrence of the hydrothermal liquefaction reaction.
  • a filter screen is provided on the top of the first baffle cylinder, and the slag cleaning mechanism extends into the first baffle cylinder through the filter screen to achieve separation of solid phase products in the hydrothermal liquefaction product.
  • the slag cleaning mechanism includes a motor, a rotating shaft, a slag scraping device and a salt scraping device; one end of the rotating shaft is equipped with the motor, and the other end extends into the first baffle cylinder through the filter screen, and the slag scraping device and the salt scraping device are respectively installed on the rotating shaft in the first baffle cylinder, so as to realize continuous and efficient operation of the filter screen and reduce salt deposition on the inner wall of the reactor.
  • a microwave controller is provided on the first-stage hydrothermal liquefaction chamber, and a plurality of microwave generators are provided on both the first-stage hydrothermal liquefaction chamber and the second-stage hydrothermal liquefaction chamber to assist the hydrothermal liquefaction reaction and improve the yield and quality of the bio-crude oil.
  • FIG1 is a schematic structural diagram of a reactor of the present invention.
  • the purpose of the present invention is to provide a two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device to solve the technical problems in the prior art that the mixing efficiency of multiple materials and media is low; the material mixer, reactor, solid phase product filter, and heat recovery of hydrothermal liquefaction are separate and complex in structure, making it impossible to achieve two-stage hydrothermal liquefaction; and the presence of biomass with excessively high temperature and salt deposition that seriously clogs the pipeline.
  • the two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device includes a first-stage hydrothermal liquefaction chamber 19, a second-stage hydrothermal liquefaction chamber 10 and a medium-temperature hydrothermal transition product collection box 18; a plurality of material feed ports and medium feed ports 30 are provided on one side of the top of the first-stage hydrothermal liquefaction chamber 19, a high-temperature hydrothermal product feed port 3 is provided on the other side of the top, a hydrothermal final product discharge port 22 is provided on the bottom, and a plurality of first-stage hydrothermal liquefaction reaction tubes 20 are longitudinally provided inside, and the plurality of first-stage hydrothermal liquefaction reaction tubes 20 are connected in sequence, and one end of each first-stage hydrothermal liquefaction reaction tube 20 extends through the inner wall of the first-stage hydrothermal liquefaction chamber 19 and is connected to the input end of the medium-temperature hydrothermal transition product collection box 18,
  • a nozzle 28 is provided between the plurality of material feed ports and the medium feed port 30 and one end of the first stage hydrothermal liquefaction reaction tube 20 at the top, wherein one end of the nozzle 28 is provided with multiple pipelines, which are sequentially connected to It should be connected to several material feed ports and medium feed ports 30 , and the other end of the nozzle 28 is a single pipeline, which is connected to one end of the first-stage hydrothermal liquefaction reaction tube 20 .
  • a receiving tube 27, a mixing tube 26 and a diffusion tube 31 are arranged in sequence between the single pipeline and one end of the first-stage hydrothermal liquefaction reaction tube 20, wherein the receiving tube 27, the mixing tube 26 and the diffusion tube 31 are all of different diameter structures.
  • each first-stage hydrothermal liquefaction reaction tube 20 is provided with an inclination angle of 1-3°.
  • a high-temperature and high-pressure needle valve 23 is provided at one end of each first-stage hydrothermal liquefaction reaction tube 20 close to the medium-temperature hydrothermal transition product collection box 18 and between each first-stage hydrothermal liquefaction reaction tube 20 .
  • an electric heating coil 8 is provided between the second insulation layer 9 and the outer wall of the second-stage hydrothermal liquefaction chamber 10 .
  • a filter screen 6 is provided on the top of the first baffle cylinder 7 , and the slag cleaning mechanism extends into the first baffle cylinder 7 through the filter screen 6 .
  • the slag cleaning mechanism includes a motor 5, a rotating shaft, a slag scraping device 11 and a salt scraping device 15; one end of the rotating shaft is equipped with the motor 5, and the other end extends into the first baffle cylinder 7 through the filter 6, and the slag scraping device 11 and the salt scraping device 15 are respectively assembled on the rotating shaft in the first baffle cylinder 7.
  • a microwave controller 21 is provided on the first-stage hydrothermal liquefaction chamber 19, and a plurality of microwave generators 24 are provided on both the first-stage hydrothermal liquefaction chamber 19 and the second-stage hydrothermal liquefaction chamber 10.
  • This embodiment provides a microwave-assisted integrated two-stage co-liquefaction mixing-reaction-filtration device with precise reaction time control, comprising:
  • It includes a first-stage hydrothermal liquefaction generating chamber 19 and a second-stage hydrothermal liquefaction generating chamber 10;
  • the first stage hydrothermal liquefaction chamber 19 is provided with a first insulation layer 2 on the outer layer, a first stage hydrothermal liquefaction reaction tube 20 is provided inside, a material first feed port 1, a material second feed port 29 and a medium feed port 30 are provided on the upper left side, a high temperature hydrothermal product feed port 3 is provided on the upper right side, and a hydrothermal final product discharge port 22 is provided on the lower left side;
  • the second stage hydrothermal liquefaction chamber 10 is provided with a second insulation layer 9 and an electric heating coil 8 from the outside to the inside, and a coaxial first baffle/tube 7 and a second baffle/tube 13 are provided inside to transfer the second stage hydrothermal liquid
  • the reaction zone of the liquefaction chamber is divided into a heating zone, a catalytic zone and an insulation zone.
  • a filter screen 7 is provided on the upper side of the interior to separate the solid phase products from the hydrothermal liquefaction products.
  • a high-temperature hydrothermal product discharge port 4 is provided on the top, and a second slag discharge port 16 and a first slag discharge port 14 are provided in the middle and right side of the bottom.
  • the reaction zone between the inner wall of the second stage hydrothermal liquefaction chamber 10 and the second baffle cylinder 13 is the heating zone, which heats the temperature from 150-250°C to 300-350°C.
  • the reaction zone between the second baffle cylinder 13 and the first flow cylinder 7 is the catalytic zone, in which a catalyst grid 12 is provided to store the hydrothermal liquefaction heterogeneous catalyst.
  • the reaction zone inside the first flow plate/cylinder 7 is the insulation zone, in which the material is maintained at 300-350°C for hydrothermal liquefaction reaction.
  • a motor 5 is provided outside the hydrothermal liquefaction chamber of the second stage, which drives a scraper device 11 and a salt scraper device 15 fixed on the shaft and arranged in the heat preservation zone to rotate through a rotating shaft, so as to scrape off the filter residue and salt deposited on the inner wall of the reactor and the filter screen.
  • the first-stage hydrothermal liquefaction chamber 19 has a medium-temperature hydrothermal transition product collecting box 18, a high-temperature and high-pressure needle valve 23, and a medium-temperature hydrothermal transition product discharge port 25.
  • the outflow of the first-stage hydrothermal liquefaction product is controlled by opening and closing the high-temperature and high-pressure needle valve, thereby achieving precise control of the first-stage hydrothermal liquefaction reaction time.
  • the outflowing medium-temperature hydrothermal liquefaction product is collected in the medium-temperature hydrothermal transition product collecting box 18, and then enters the second-stage hydrothermal liquefaction chamber through the medium-temperature hydrothermal transition product feed port to produce a more intense hydrothermal liquefaction reaction.
  • a nozzle 28, a receiving chamber 27, a mixing chamber 26 and a diffusion chamber 31 are arranged between the material and medium feed ports and the first-stage hydrothermal liquefaction reaction tube 20 to achieve sufficient mixing of the first material, the second material and the medium.
  • the first stage hydrothermal liquefaction reaction tube is set with an inclination angle of 1-3°.
  • a microwave controller 21 and a microwave generator 24 are arranged outside the reactor to assist the hydrothermal liquefaction reaction and improve the yield and quality of the bio-crude oil.
  • the two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device provided by the present invention is used:
  • the microalgae and sludge When the microalgae and sludge are hydrothermally liquefied together, they enter the first stage hydrothermal liquefaction chamber 19 from the first material feed port 1 and the second material feed port 2 respectively, and the water medium enters the first stage hydrothermal liquefaction chamber 19 from the medium inlet, so that the sludge, microalgae and water reach a suitable ratio.
  • the first-stage hydrothermal liquefaction reaction tube 20 descends and is heated by the medium heat from the second-stage hydrothermal liquefaction chamber 10, with the temperature reaching 150-250°C, to generate a medium-temperature hydrothermal liquefaction reaction.
  • the medium-temperature hydrothermal transition product is discharged from the medium-temperature hydrothermal transition product outlet 25 through the high-temperature and high-pressure needle valve 23, and flows into the second-stage hydrothermal liquefaction chamber 10 for a high-temperature hydrothermal liquefaction reaction.
  • the slurry entering the second-stage hydrothermal liquefaction chamber 10 through the medium-temperature hydrothermal transition product feed port 17 is first heated in the reaction zone, and the temperature is raised to 350°C by the electric heating coil 8, and then returns to the catalytic reaction zone through the baffle tube, and through the catalytic grid set in the reaction zone, the organic compound is efficiently converted under the action of the heterogeneous catalyst.
  • the slurry reaching the bottom is once again returned under the action of the baffle plate, and after the solid phase in the product is filtered through the filter screen 6 at the top, it is discharged from the high-temperature hydrothermal product discharge port 4 on the upper left side, enters the first-stage hydrothermal liquefaction chamber 19 to heat the entering slurry, and finally is discharged from the hydrothermal final product discharge port 22 on the lower left side of the first-stage hydrothermal liquefaction chamber 19.
  • the motor 5 above the second-stage hydrothermal liquefaction chamber 10 drives the scraper device 11 and the salt scraper device 15 in the second-stage hydrothermal liquefaction chamber 10 to rotate, clean the filter residue and salt layer deposited on the inner wall of the reactor and the filter screen 6, and discharge them from the slag discharge port at the bottom after the reaction is completed.
  • the present invention provides a two-stage co-liquefaction mixing-reaction-filtration-heat recovery integrated device, which realizes the realization of the two-stage hydrothermal liquefaction process; secondly, nozzles, receiving chambers, mixing chambers and diffusion chambers are set at the inlets of different materials and media, and high-speed fluids are collided and mixed in these structures; thirdly, the heat of hydrothermal liquefaction in the first stage comes from the heat of the hydrothermal liquefaction product in the second stage, and at the same time, the occurrence of the hydrothermal liquefaction reaction in the first stage and the recovery rate of the heat of the hydrothermal liquefaction product in the second stage are realized, thereby improving the economy; thirdly, in the first stage hydrothermal liquefaction process, the high-temperature and high-pressure needle valve is set to achieve precise control of different reaction times, so as to select different first stage hydrothermal liquefaction reaction times according to different material characteristics; finally, the first stage hydrothermal liquef
  • the device is a highly integrated device, which realizes the coupling of mixing, reaction, filtration and heat recovery processes, greatly reduces the complexity and construction cost of the system, and utilizes the co-hydration
  • the new liquefaction process of thermal liquefaction and two-stage hydrothermal liquefaction has obtained high-yield and high-quality bio-crude oil, improved the economy of the system, and promoted the industrial development of hydrothermal liquefaction technology.

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Abstract

提供一种两阶段共液化混合-反应-过滤-热回收一体式装置，实现了两阶段水热液化过程的实现；其次，在不同物料及介质的进口处设置了喷嘴(28)、接受室(27)、混合室(26)和扩散室(31)，高速流体在这些结构内实现冲分的碰撞及混合；第一阶段的水热液化热量来自于第二阶段水热液化产物的热量，同时实现了第一阶段水热液化反应的发生和第二阶段水热液化产物热量的回收率用，提高了经济性；在第一阶段水热液化过程中，通过高温高压针阀(23)的设置，实现了不同反应时间的精准控制，从而针对不同的物料特性选择不同的第一阶段水热液化反应时间；第一阶段水热液化反应管(20)设置了1-3°的倾斜，第二阶段水热液化发生室(10)中设置了刮渣装置(11)和刮盐装置(15)，保障了反应器的稳定运行。

Description

一种两阶段共液化混合-反应-过滤-热回收一体式装置 技术领域
本发明涉及水热液化设备技术领域，具体为一种两阶段共液化混合-反应-过滤-热回收一体式装置。
背景技术
共水热液化是将两种或多种原料合并进行水热液化的一种方法。将不同材料混合在一起参与反应不仅可以产生简单的叠加作用，而且由于这些材料的协同或拮抗作用而产生复合效果。实验研究发现，不同物质组成之间进行共水热液化具有显著的协同作用，往往可以获得高品质和高产率的生物原油。因此，发展先进高效的共水热液化技术，高效进行生物质转化，进行生物质资源化利用，已经成为水热技术领域发展的新方向。
两阶段水热液化是的第一阶段在低温下进行水热处理，然后在更严格的条件下进行水热液化，低温水热处理的存在显著影响了最终的元素组成、HHV、能量回收率、分子组分以及水相的TOC浓度和固体产率。且潜在的能量消耗节省和反应温度降低导致了设备成本的降低，因而说明两阶段水热液化是一种理想的液化过程。
目前，设计的水热液化反应系统大多为单程的单物质水热液化反应，传统的水热液化反应器为简单的管式反应器，在使用过程中存在以下一些问题：没有适用于两阶段水热液化的反应器；水热液化的物料混合器、反应器、固相产物过滤器、热量回收为分离式的，造成系统复杂设备造价成本高的问题；生物质特别是城市污泥中存在高浓度盐及灰分，存在温度过高盐沉积严重堵塞管道的风险；简单的多个物料进口设置，物料和介质混合效率低，不同的组分分子 无法充分接触。
因此，为了解决上述问题，实现多种生物质进行两阶段的共水热液化，急需一种能够实现高效混合、进行两阶段水热液化反应、分离水热液化产物中固相的高度集成装置。
发明内容
为了克服上述现有技术存在的缺陷，本发明的目的在于提供一种两阶段共液化混合-反应-过滤-热回收一体式装置，以解决现有技术中多种物料和介质混合效率低；水热液化的物料混合器、反应器、固相产物过滤器、热量回收为分离式的结构复杂，无法实现两阶段水热液化以及生物质存在温度过高盐沉积严重堵塞管道的技术问题。
本发明是通过以下技术方案来实现：
一种两阶段共液化混合-反应-过滤-热回收一体式装置，包括第一阶段水热液化发生室、第二阶段水热液化发生室和中温水热过渡产物汇集箱；第一阶段水热液化发生室的顶部一侧设有若干物料进料口和介质进料口，顶部另一侧设有高温水热产物进料口，底部设有水热终产物出料口，内部纵向设有若干第一阶段水热液化反应管，若干第一阶段水热液化反应管之间依次相连，每个第一阶段水热液化反应管的一端均通过第一阶段水热液化发生室的内壁伸出并连接至中温水热过渡产物汇集箱的输入端，且顶端的第一阶段水热液化反应管的一端均连接若干物料进料口和介质进料口；第二阶段水热液化发生室的底端侧壁上设有中温水热过渡产物进料口，中温水热过渡产物汇集箱的输出端连接至中温水热过渡产物进料口；第二阶段水热液化发生室内沿着内壁至中心位置处同轴设有第二折流筒和第一折流筒；其中第二折流筒的外壁与第二阶段水热液化发生室的内壁之间形成加热区，第二折流筒和第一折流筒之间形成催化区设有若干催化剂栅格，第一折流筒内形成保温区，所述保温区对应的第二阶段水热液化发生室的顶部设有高温水热产物出料口，高温水热产物出料口与高温水热产物进料口连通，所述第一折流筒内设有清渣机构，所述第二阶段水热液化发 生室的底端设有第二排渣口，所述第二阶段水热液化发生室的底部外侧还设有第一排渣口。
优选的，若干物料进料口和介质进料口与顶端的第一阶段水热液化反应管的一端之间设有喷嘴，其中喷嘴的一端设有多管路，多管路依次对应连接至若干物料进料口和介质进料口，喷嘴的另一端为单管路，所述单管路与第一阶段水热液化反应管的一端连接；
所述单管路与第一阶段水热液化反应管的一端之间依次设有接收管、混合管和扩散管，其中接收管、混合管和扩散管均呈异径结构。
优选的，每个第一阶段水热液化反应管设置有1-3°的倾斜角。
优选的，每个靠近中温水热过渡产物汇集箱的第一阶段水热液化反应管一端处以及每个第一阶段水热液化反应管之间均设有高温高压针阀。
优选的，在第二保温层与第二阶段水热液化发生室的外壁之间设有电加热线圈。
优选的，第一折流筒的顶部设有滤网，清渣机构通过滤网伸入至第一折流筒内。
进一步的，清渣机构包括电机、旋转轴、刮渣装置和刮盐装置；旋转轴的一端装配电机，另一端通过滤网伸入至第一折流筒内，所述刮渣装置和刮盐装置分别装配在第一折流筒内的旋转轴上。
优选的，第一阶段水热液化发生室上设有微波控制器，且第一阶段水热液化发生室和第二阶段水热液化发生室上均设有若干微波发生器。
与现有技术相比，本发明具有以下有益的技术效果：
本发明提供了一种两阶段共液化混合-反应-过滤-热回收一体式装置，实现了两阶段水热液化过程的实现；其次，在不同物料及介质的进口处设置了喷嘴、接受室、混合室和扩散室，高速流体在这些结构内实现冲分的碰撞及混合；再次，第一阶段的水热液化热量来自于第二阶段水热液化产物的热量，同时实现了第一阶段水热液化反应的发生和第二阶段水热液化产物热量的回收率用，提 高了经济性；再次，在第一阶段水热液化过程中，通过高温高压针阀的设置，实现了不同反应时间的精准控制，从而针对不同的物料特性选择不同的第一阶段水热液化反应时间；最后，第一阶段水热液化反应管设置了1-3°的倾斜，第二阶段水热液化发生室中设置了刮渣装置和刮盐装置，保障了反应器的稳定运行。该装置是一个高度集成装置，实现了混合、反应、过滤、热回收过程的耦合，极大程度的减少了系统的复杂程度和建造成本，利用了共水热液化和两阶段水热液化的新型液化流程，获得了高产率和高品质的生物原油，提高了系统的经济性，促进了水热液化技术的产业化发展。
进一步的，若干物料进料口和介质进料口与顶端的第一阶段水热液化反应管的一端之间设有喷嘴，其中喷嘴的一端设有多管路，多管路依次对应连接至若干物料进料口和介质进料口，喷嘴的另一端为单管路，所述单管路与第一阶段水热液化反应管的一端连接，单管路与第一阶段水热液化反应管的一端之间依次设有接收管、混合管和扩散管，其中接收管、混合管和扩散管均呈异径结构，提高了对若干物料和介质之间的混合效率。
进一步的，每个靠近中温水热过渡产物汇集箱的第一阶段水热液化反应管一端处以及每个第一阶段水热液化反应管之间均设有高温高压针阀，通过高温高压针阀的启闭控制第一阶段水热液化产物的流出，实现第一阶段水热液化反应时间的精准控制。
进一步的，第二折流筒和第一折流筒之间的催化区内设有若干催化剂栅格，有效的促进水热液化反应的发生。
进一步的，第一折流筒的顶部设有滤网，清渣机构通过滤网伸入至第一折流筒内，实现水热液化产物中固相产物的分离。
进一步的，清渣机构包括电机、旋转轴、刮渣装置和刮盐装置；旋转轴的一端装配电机，另一端通过滤网伸入至第一折流筒内，所述刮渣装置和刮盐装置分别装配在第一折流筒内的旋转轴上，实现滤网的持续高效工作和减少反应器内壁的盐沉积情况。
进一步的，第一阶段水热液化发生室上设有微波控制器，且第一阶段水热液化发生室和第二阶段水热液化发生室上均设有若干微波发生器，辅助水热液化反应进行，提高生物原油产率及品质。
附图说明
图1为本发明反应器的结构简图。
图中：1-第一物料进料口；2-第一保温层；3-高温水热产物进料口；4-高温水热产物出料口；5-电机；6-滤网；7-第一折流筒；8-电加热线圈；9-第二保温层；10-第二阶段水热液化发生室；11-刮渣装置；12-催化剂栅格；13-第二折流筒；14-第一排渣口；15-刮盐装置；16-第二排渣口；17-中温水热过渡产物进料口；18-中温水热过渡产物汇集箱；19-第一阶段水热液化发生室；20-第一阶段水热液化反应管；21-微波控制器；22-水热终产物出料口；23-高温高压针阀；24-微波发生器；25-中温水热过渡产物出料口；26-混合管；27-接收管；28-喷嘴；29-第二物料进料口；30-介质进料口；31-扩散管。
具体实施方式
为了使本技术领域的人员更好地理解本发明方案，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分的实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都应当属于本发明保护的范围。
需要说明的是，本发明的说明书和权利要求书及上述附图中的术语“第一”、“第二”等是用于区别类似的对象，而不必用于描述特定的顺序或先后次序。应该理解这样使用的数据在适当情况下可以互换，以便这里描述的本发明的实施例能够以除了在这里图示或描述的那些以外的顺序实施。此外，术语“包括”和“具有”以及他们的任何变形，意图在于覆盖不排他的包含，例如，包含了一系列步骤或单元的过程、方法、系统、产品或设备不必限于清楚地列出的那些步骤或单元，而是可包括没有清楚地列出的或对于这些过程、方法、产品或设备 固有的其它步骤或单元。
下面结合附图对本发明做进一步详细描述：
本发明的目的在于提供一种两阶段共液化混合-反应-过滤-热回收一体式装置，以解决现有技术中多种物料和介质混合效率低；水热液化的物料混合器、反应器、固相产物过滤器、热量回收为分离式的结构复杂，无法实现两阶段水热液化以及生物质存在温度过高盐沉积严重堵塞管道的技术问题。
具体的，根据图1所示，该两阶段共液化混合-反应-过滤-热回收一体式装置，包括第一阶段水热液化发生室19、第二阶段水热液化发生室10和中温水热过渡产物汇集箱18；第一阶段水热液化发生室19的顶部一侧设有若干物料进料口和介质进料口30，顶部另一侧设有高温水热产物进料口3，底部设有水热终产物出料口22，内部纵向设有若干第一阶段水热液化反应管20，若干第一阶段水热液化反应管20之间依次相连，每个第一阶段水热液化反应管20的一端均通过第一阶段水热液化发生室19的内壁伸出并连接至中温水热过渡产物汇集箱18的输入端，且顶端的第一阶段水热液化反应管20的一端均连接若干物料进料口和介质进料口30；第二阶段水热液化发生室10的底端侧壁上设有中温水热过渡产物进料口17，中温水热过渡产物汇集箱18的输出端连接至中温水热过渡产物进料口17；第二阶段水热液化发生室10内沿着内壁至中心位置处同轴设有第二折流筒13和第一折流筒7；其中第二折流筒13的外壁与第二阶段水热液化发生室10的内壁之间形成加热区，第二折流筒13和第一折流筒7之间形成催化区设有若干催化剂栅格12，第一折流筒7内形成保温区，所述保温区对应的第二阶段水热液化发生室10的顶部设有高温水热产物出料口4，高温水热产物出料口4与高温水热产物进料口3连通，所述第一折流筒7内设有清渣机构，所述第二阶段水热液化发生室10的底端设有第二排渣口16，所述第二阶段水热液化发生室10的底部外侧还设有第一排渣口14。
具体的，若干物料进料口和介质进料口30与顶端的第一阶段水热液化反应管20的一端之间设有喷嘴28，其中喷嘴28的一端设有多管路，多管路依次对 应连接至若干物料进料口和介质进料口30，喷嘴28的另一端为单管路，所述单管路与第一阶段水热液化反应管20的一端连接。
其中，单管路与第一阶段水热液化反应管20的一端之间依次设有接收管27、混合管26和扩散管31，其中接收管27、混合管26和扩散管31均呈异径结构。
具体的，每个第一阶段水热液化反应管20设置有1-3°的倾斜角。
具体的，每个靠近中温水热过渡产物汇集箱18的第一阶段水热液化反应管20一端处以及每个第一阶段水热液化反应管20之间均设有高温高压针阀23。
具体的，在第二保温层9与第二阶段水热液化发生室10的外壁之间设有电加热线圈8。
具体的，第一折流筒7的顶部设有滤网6，清渣机构通过滤网6伸入至第一折流筒7内。
其中，清渣机构包括电机5、旋转轴、刮渣装置11和刮盐装置15；旋转轴的一端装配电机5，另一端通过滤网6伸入至第一折流筒7内，所述刮渣装置11和刮盐装置15分别装配在第一折流筒7内的旋转轴上。
具体的，第一阶段水热液化发生室19上设有微波控制器21，且第一阶段水热液化发生室19和第二阶段水热液化发生室10上均设有若干微波发生器24，
实施例
本实施例提供了一种微波辅助的一体式精准控制反应时间的两阶段共液化的混合-反应-过滤装置，包括：
包括第一阶段水热液化发生室19和第二阶段水热液化发生室10；
第一阶段水热液化发生室19外层设有第一保温层2，内部设有第一阶段水热液化反应管20，左上侧设有物料一进料口1、物料二进料口29和介质进料口30，右上侧设有高温水热产物进料口3，左下侧设有水热终产物出料口22；
第二阶段水热液化发生室10从外到内依次设有第二保温层9和电加热线圈8，内部设有同轴的第一折流板/筒7和第二折流板/筒13将第二阶段水热液 化发生室反应区分割为加热区、催化区和保温区，内部上侧设有滤网7，实现水热液化产物中固相产物的分离，顶部设有高温水热产物出料口4，底部中间和右侧设有第二排渣口16和第一排渣口14。
第二阶段水热液化发生室10内壁与第二折流筒13之间的反应区为加热区，将温度从150-250℃加热到300-350℃，第二折流筒13与第一流筒7之间的反应区为催化区，设置有催化剂栅格12存放水热液化非均相催化剂，第一流板/筒7内部的反应区为保温区，物料在该区域内维持在300-350℃发生水热液化反应。
第二阶段水热液化发生室外侧设有电机5，通过一根旋转轴带动轴上固定的设置在保温区内的刮渣装置11和刮盐装置15旋转，刮下反应器内壁和滤网上沉积的滤渣和盐。
第一阶段水热液化发生室19中温水热过渡产物汇集箱18、高温高压针阀23、中温水热过渡产物出料口25，通过高温高压针阀的启闭控制第一阶段水热液化产物的流出，实现第一阶段水热液化反应时间的精准控制，流出的中温水热液化产物汇集到中温水热过渡产物汇集箱18中，随后通过中温水热过渡产物进料口进入到第二阶段水热液化发生室，发生强度更大的水热液化反应。
在物料及介质进料口以及第一阶段水热液化反应管20之间设置有喷嘴28、接受室27、混合室26、扩散室31，实现物料一、物料二以及介质的充分混合。
第一阶段水热液化反应管设置有1-3°的倾斜角。
反应器外部设置有微波控制器21和微波发生器24，辅助水热液化反应进行，提高生物原油产率及品质。
本发明所提供的一种两阶段共液化混合-反应-过滤-热回收一体式装置在使用时：
微藻及污泥共水热液化时，分别从第一物料进料口1和第二物料进料口2进入到第一阶段水热液化发生室19，水介质从介质进口进入到第一阶段水热液化发生室19，使得污泥、微藻及水达到合适的比例。混合后的反应物浆料沿第 一阶段水热液化反应管20下降，利用从第二阶段水热液化发生室10出来的介质热量进行加热，温度道道150-250℃，发生中温水热液化反应。20min后，达到需要的第一阶段反应时间后，中温水热过渡产物从中温水热过渡产物出料口25经高温高压针阀23控制排出，流入到第二阶段水热液化发生室10进行高温水热液化反应。
经中温水热过渡产物进料口17进入到第二阶段水热液化发生室10的浆料首先在加热反应区，利用电加热线圈8实现温度升高至350℃，随后经折流筒作用折返进入到催化反应区，通过设置在反应区内的催化栅格，在非均相催化剂的作用下，实现有机化合物的高效转化。到达底部的浆料在折流板的作用下再一次折返，经顶部的滤网6过滤产物中的固相后，从左上侧的高温水热产物出料口4排出，进入到第一阶段水热液化发生室19对进入的浆料进行加热，最后从第一阶段水热液化发生室19左下侧的水热终产物出料口22排出。
整个过程中，第二阶段水热液化发生室10上方的电机5带动第二阶段水热液化发生室10中的刮渣装置11和刮盐装置15旋转，对反应器内壁及滤网6上沉积的滤渣和盐层进行清扫，并在结束反应后从底部的排渣口排出。
综上所述，本发明提供了一种两阶段共液化混合-反应-过滤-热回收一体式装置，实现了两阶段水热液化过程的实现；其次，在不同物料及介质的进口处设置了喷嘴、接受室、混合室和扩散室，高速流体在这些结构内实现冲分的碰撞及混合；再次，第一阶段的水热液化热量来自于第二阶段水热液化产物的热量，同时实现了第一阶段水热液化反应的发生和第二阶段水热液化产物热量的回收率用，提高了经济性；再次，在第一阶段水热液化过程中，通过高温高压针阀的设置，实现了不同反应时间的精准控制，从而针对不同的物料特性选择不同的第一阶段水热液化反应时间；最后，第一阶段水热液化反应管设置了1-3°的倾斜，第二阶段水热液化发生室中设置了刮渣装置和刮盐装置，保障了反应器的稳定运行。该装置是一个高度集成装置，实现了混合、反应、过滤、热回收过程的耦合，极大程度的减少了系统的复杂程度和建造成本，利用了共水 热液化和两阶段水热液化的新型液化流程，获得了高产率和高品质的生物原油，提高了系统的经济性，促进了水热液化技术的产业化发展。
最后应当说明的是：以上实施例仅用以说明本发明的技术方案而非对其限制，尽管参照上述实施例对本发明进行了详细的说明，所属领域的普通技术人员应当理解：依然可以对本发明的具体实施方式进行修改或者等同替换，而未脱离本发明精神和范围的任何修改或者等同替换，其均应涵盖在本发明的权利要求保护范围之内。

Claims (8)

  1. 一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，包括第一阶段水热液化发生室(19)、第二阶段水热液化发生室(10)和中温水热过渡产物汇集箱(18)；第一阶段水热液化发生室(19)的顶部一侧设有若干物料进料口和介质进料口(30)，顶部另一侧设有高温水热产物进料口(3)，底部设有水热终产物出料口(22)，内部纵向设有若干第一阶段水热液化反应管(20)，若干第一阶段水热液化反应管(20)之间依次相连，每个第一阶段水热液化反应管(20)的一端均通过第一阶段水热液化发生室(19)的内壁伸出并连接至中温水热过渡产物汇集箱(18)的输入端，且顶端的第一阶段水热液化反应管(20)的一端均连接若干物料进料口和介质进料口(30)；第二阶段水热液化发生室(10)的底端侧壁上设有中温水热过渡产物进料口(17)，中温水热过渡产物汇集箱(18)的输出端连接至中温水热过渡产物进料口(17)；第二阶段水热液化发生室(10)内沿着内壁至中心位置处同轴设有第二折流筒(13)和第一折流筒(7)；其中第二折流筒(13)的外壁与第二阶段水热液化发生室(10)的内壁之间形成加热区，第二折流筒(13)和第一折流筒(7)之间形成催化区设有若干催化剂栅格(12)，第一折流筒(7)内形成保温区，所述保温区对应的第二阶段水热液化发生室(10)的顶部设有高温水热产物出料口(4)，高温水热产物出料口(4)与高温水热产物进料口(3)连通，所述第一折流筒(7)内设有清渣机构，所述第二阶段水热液化发生室(10)的底端设有第二排渣口(16)，所述第二阶段水热液化发生室(10)的底部外侧还设有第一排渣口(14)。
  2. 根据权利要求1所述的一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，若干物料进料口和介质进料口(30)与顶端的第一阶段水热液化反应管(20)的一端之间设有喷嘴(28)，其中喷嘴(28)的一端设有多管路，多管路依次对应连接至若干物料进料口和介质进料口(30)，喷嘴(28)的另一端为单管路，所述单管路与第一阶段水热液化反应管(20)的一端连接；
    所述单管路与第一阶段水热液化反应管(20)的一端之间依次设有接收管(27)、混合管(26)和扩散管(31)，其中接收管(27)、混合管(26)和扩散 管(31)均呈异径结构。
  3. 根据权利要求1所述的一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，每个第一阶段水热液化反应管(20)设置有1-3°的倾斜角。
  4. 根据权利要求1所述的一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，每个靠近中温水热过渡产物汇集箱(18)的第一阶段水热液化反应管(20)一端处以及每个第一阶段水热液化反应管(20)之间均设有高温高压针阀(23)。
  5. 根据权利要求1所述的一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，在第二保温层(9)与第二阶段水热液化发生室(10)的外壁之间设有电加热线圈(8)。
  6. 根据权利要求1所述的一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，所述第一折流筒(7)的顶部设有滤网(6)，清渣机构通过滤网(6)伸入至第一折流筒(7)内。
  7. 根据权利要求6所述的一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，所述清渣机构包括电机(5)、旋转轴、刮渣装置(11)和刮盐装置(15)；旋转轴的一端装配电机(5)，另一端通过滤网(6)伸入至第一折流筒(7)内，所述刮渣装置(11)和刮盐装置(15)分别装配在第一折流筒(7)内的旋转轴上。
  8. 根据权利要求1所述的一种两阶段共液化混合-反应-过滤-热回收一体式装置，其特征在于，所述第一阶段水热液化发生室(19)上设有微波控制器(21)，且第一阶段水热液化发生室(19)和第二阶段水热液化发生室(10)上均设有若干微波发生器(24)。
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