WO2021237512A1 - 一种用于材料的多功能超临界流体处理机 - Google Patents

一种用于材料的多功能超临界流体处理机 Download PDF

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Publication number
WO2021237512A1
WO2021237512A1 PCT/CN2020/092620 CN2020092620W WO2021237512A1 WO 2021237512 A1 WO2021237512 A1 WO 2021237512A1 CN 2020092620 W CN2020092620 W CN 2020092620W WO 2021237512 A1 WO2021237512 A1 WO 2021237512A1
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Prior art keywords
fluid
processing
puffing
carbon dioxide
temperature
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PCT/CN2020/092620
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English (en)
French (fr)
Inventor
龙家杰
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南通纺织丝绸产业技术研究院
苏州大学
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Priority to PCT/CN2020/092620 priority Critical patent/WO2021237512A1/zh
Publication of WO2021237512A1 publication Critical patent/WO2021237512A1/zh

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves

Definitions

  • the present invention relates to a multifunctional supercritical fluid processing machine for materials, which belongs to the technical fields of manufacturing pressure vessels, textile dyeing and finishing, material processing, food and feed and other processing equipment. Background technique
  • Materials processing such as expansion, foaming, and fragmentation have important applications in industrial and agricultural fields such as textiles, food, building materials, crop by-product processing, feed, new material manufacturing, chemical engineering, aerospace, medical and health care.
  • the original structure and volume of the material can be changed relatively easily, and the material can be given diversified functions or characteristics.
  • material can be reduced in weight, and the material's thermal insulation, morphological stability, and stress-strain characteristics can be improved.
  • it can improve the processability, digestion and absorption characteristics, utilization efficiency of raw materials, and improve the nutritional properties and taste or flavor of food.
  • the supercritical carbon dioxide fluid medium has received extensive attention in the field of material processing in recent years.
  • the medium has excellent biocompatibility, is colorless, odorless, non-flammable, non-explosive, non-toxic, and has remarkable ecological and environmental protection characteristics.
  • its critical point 31.1° C and 7.38MPa
  • the supercritical fluid of the medium has low viscosity, good diffusibility, permeability and penetration, and it is easy to achieve alignment.
  • Dense solid materials, hydrophobic materials, or difficult-to-penetrate and difficult-to-penetrate processing materials are highly efficient. At the same time, it is also suitable for processing various hydrophilic materials and various inorganic materials. And it can effectively shorten the process time and reduce the cost.
  • the processing there is no need to use and consume water resources, and the processed material is in a dry state; the medium is also very easy to separate, recover and recycle after the process is completed, and there are no harmful and harmful substances or other magazine residues on the processed product. After the processing is completed, the product No drying is required.
  • the existing literature there is currently no relevant report on the multifunctional equipment that uses supercritical carbon dioxide fluid medium to realize the processing and processing of material expansion, foaming, and fragmentation. Summary of the inventionTechnical problemsProblem solutionsTechnical solutions
  • the present invention provides a supercritical carbon dioxide fluid with high efficiency, wide applicability, simple operation, stable system, clean and environmentally friendly, and no noise impact, etc., which can effectively achieve supercritical carbon dioxide fluid for various materials Multifunctional supercritical fluid processing machine for puffing and other processing.
  • the technical solution adopted to achieve the objective of the present invention is to provide a multifunctional supercritical fluid processor for materials, which includes a high-temperature and high-pressure fluid puffing processing system, a carbon dioxide medium pressurization system, and an auxiliary medium pressurization system , Circulating processing system, carbon dioxide separation and recovery system and auxiliary medium separation and recovery system;
  • the high temperature and high pressure fluid puffing processing system includes a high temperature and high pressure fluid processing zone and a fluid puffing buffer zone, the high temperature and high pressure fluid puffing processing system and the circulating processing system
  • One end of the circulating treatment system is connected to the carbon dioxide separation and recovery system, and the other end is connected to the carbon dioxide medium pressurization system;
  • one end of the auxiliary medium pressurization system is connected to the circulating treatment system, and the other end is connected to the carbon dioxide separation and recovery system;
  • the system is connected with the carbon dioxide medium pressurization system.
  • the top of the high-temperature and high-pressure fluid treatment zone is a charging port with a quick-opening structure sealing cover.
  • the interior of the high-temperature and high-pressure fluid treatment zone is provided with a stirring mechanism, the upper part is provided with a fluid inlet, and the lower part is provided with a fluid outlet.
  • the bottom is provided with an outlet channel; the top of the fluid puffing buffer zone is provided with an inlet channel, the upper part is provided with a high-pressure window, and the lower part is provided with a hand hole with a quick opening structure.
  • the porous mesh plate or the receiving plate is placed at the lower part of the fluid puffing buffer , There is an outlet at the bottom, which is connected to the filter and the shut-off valve through a pipeline; high temperature and high pressure fluid treatment
  • the outlet channel at the bottom of the zone communicates with the inlet channel at the top of the fluid puffing buffer zone through a quick-opening valve.
  • Heating devices are respectively provided around the high temperature and high pressure fluid treatment zone and the fluid puffing buffer zone;
  • the stirring mechanism includes a magnetic stirring rotor and a magnetic stirring magnetic cylinder, the magnetic stirring magnetic cylinder is fixed on the sealing cover of the quick opening structure; the quick opening structure is sealed
  • the cover and the top of the fluid puffing buffer area are respectively equipped with pressure gauge, temperature gauge and sensor interface; quick-opening valve is one of ball valve, gate valve, plunger valve, the opening time of the valve opening from 0 to 100% is 0. 070s ⁇ 10s.
  • the present invention provides a multi-functional supercritical carbon dioxide fluid flash detonator for materials
  • the carbon dioxide medium pressurization system includes a CO 2 storage tank, a mass flow meter, a heat exchanger and a booster pump
  • the circulation processing system includes a two-way fluid medium circulation pump, a heat exchanger, and a flow meter
  • the carbon dioxide separation and recovery system includes a heat exchanger, a pressure relief pump, a separation unit, a filter, a condenser and a carbon dioxide storage tank; in the working state, The gas in the fluid flash explosion system is separated and recovered to 1. 01 X 10 5 Pa.
  • the present invention provides a multifunctional supercritical carbon dioxide fluid flash detonator for materials, the high temperature and high pressure fluid treatment zone, the temperature reaches 180 ° C or above, the pressure reaches 30 MPa or above; its fluid expansion buffer zone, The temperature reaches _50 ° C ⁇ 150 ° C or above, and the pressure reaches (X IMPa ⁇ 20MPa or above.
  • the multifunctional supercritical fluid flash detonator for materials provided by the present invention is suitable for processing materials, which can be textile fiber materials and their products, as well as various synthetic or natural polymer organic materials, or various types of Inorganic materials can also be various composite materials, or food, feed, and crop by-product materials.
  • the auxiliary medium used can be composed of one or two or more components, and can be a polar solvent medium, or other non-polar medium such as various non-polar solvents.
  • the present invention has the following significant advantages:
  • the multifunctional super-pro fluid processing machine for materials provided by the present invention can effectively achieve various types of The uniform and efficient treatment of the high-temperature, high-pressure supercritical fluid of the material is also conducive to the diffusion and penetration of the fluid medium into the material, especially for solid materials with tight texture and high diffusion resistance.
  • the quick-opening valve and fluid puffing buffer set up in the puffing processing system can effectively control the valve opening and opening rate, as well as the temperature and pressure in the final state of the treatment, so as to adjust and achieve different processes and different degrees of materials.
  • Puffing, foaming Processing such as, fragmentation, etc., which expands the functional diversity and application range of the equipment.
  • the present invention is equipped with an auxiliary medium pressurization system, a carbon dioxide medium pressurization system, a carbon dioxide separation and recovery system, and an auxiliary medium separation and recovery system in the system configuration, which can be used in the high temperature and high pressure fluid puffing processing system and its circulation processing system , Realize the processing and processing of single or comprehensive expansion of one or more mixed fluid media in any ratio.
  • the polar or non-polar medium in the auxiliary medium pressurization system can be used, which not only easily realizes the pretreatment before processing such as expanding the material, but also realizes the treatment of carbon dioxide fluid in the high temperature and high pressure processing process.
  • the polarity of the medium is adjusted in real time.
  • the use of the polar medium in the auxiliary medium pressurization system can significantly improve the processing effect of highly polar materials, such as hydrophilic or hydrophilic materials.
  • the two-way auxiliary medium booster pump provided in the auxiliary medium booster system of the present invention can greatly improve the material loading efficiency of the high-temperature and high-pressure fluid puffing processing system when negative pressure is formed when running in the reverse direction.
  • the equipped carbon dioxide separation and recovery system and auxiliary medium separation and recovery system can realize the high-efficiency separation and recovery of various mixed fluid media after the processing is completed, improve the recycling efficiency of the media, and can realize direct opening at atmospheric pressure. Greatly improve the operating efficiency and economic benefits of the equipment.
  • the technical solution provided by the present invention can realize the processing of multiple functional processing such as expansion, foaming, and fragmentation of materials, and is applicable to the processing of different polarities and different types of organic or inorganic materials.
  • taking advantage of the low viscosity, high permeability and strong penetrability of the supercritical carbon dioxide fluid medium components it is easy to realize the processing and processing of dense solids and hard-to-permeate materials. This is of great significance to the development of green, ecological and safe processing of related materials, and it also has very broad application prospects. Therefore, using these unique advantages of the supercritical carbon dioxide fluid medium for processing various materials such as expansion, foaming, and fragmentation has broad market prospects.
  • FIG. 1 is a schematic diagram of the system structure of a multifunctional supercritical fluid processing machine for materials provided by an embodiment of the present invention
  • FIG. 2 is a schematic cross-sectional structure diagram of a high temperature and high pressure fluid puffing processing system provided by an embodiment of the present invention.
  • FIG. 1 In Figure 1: 1. C0 2 storage tank; 2 (3, 10, 24, 27), stop valve; 4. booster pump; 5. mass flow meter; 6 (11, 13, 17, 18, 22, 25), solenoid valve; 7 (19), heat exchanger; 8, body Accumulative flow meter; 9. Two-way fluid medium circulation pump; 12. High temperature and high pressure fluid puffing processing system; 14. Auxiliary medium mass flow meter; 15. Two-way auxiliary medium booster pump; 16. Auxiliary medium evaporator and storage unit; 20. Pressure relief pump; 21. Mixed media separation unit; 23. Filter; 26. Condenser; 28. CO 2 gas inlet.
  • FIG. 2 12-1, fluid inlet; 12-1', fluid outlet; 12-2 (12-2', 12-16), stop valve; 12-3, magnetic stirring rotor; 12-4 , Quick opening structure; 12-5, magnetic stirring cylinder; 12-6, pressure sensor/pressure gauge interface; 12-7, temperature sensor interface; 12-8 (12-8'), heating jacket; 12-9, High temperature and high pressure fluid processing zone; 12-10, quick opening valve; 12-11, fluid puffing buffer zone; 12-12, high pressure window; 12-13, hand hole quick opening structure in puffing processing zone; 12-14, perforated mesh plate Or receiving board; 12-15, filter.
  • This embodiment provides a multifunctional supercritical fluid processor for materials.
  • the applicable materials processed can be textile fiber materials and their products, as well as various synthetic or natural polymer organic materials, or various types of Inorganic materials can also be various composite materials, or food, feed, and crop by-product materials.
  • FIG. 1 it is a schematic diagram of the system structure of a multifunctional supercritical fluid processing machine for materials provided in this embodiment; it includes a high temperature and high pressure fluid puffing processing system, a carbon dioxide medium pressurization system, and an auxiliary medium pressurization System, recycling treatment system, carbon dioxide separation and recovery system and auxiliary medium separation and recovery system.
  • the specific structure is as follows:
  • the carbon dioxide medium pressurization system is connected to the CO 2 storage tank 1 by the CO 2 gas inlet 28 with a shut-off valve 27 , the bottom outlet of the CO 2 storage tank 1 is equipped with a shut-off valve 2, and the outlet end of the CO 2 storage tank 1 passes through the shut-off valve 3.
  • the booster pump 4 Connect the booster pump 4, the mass flow meter 5, the solenoid valve 6, and the heat exchanger 7 in sequence, and then communicate with the fluid inlet end of the high temperature and high pressure fluid puffing processing system 12 through the volume flow meter 8.
  • the auxiliary medium pressurization system is sequentially connected to the two-way auxiliary medium pressurization pump 15, the auxiliary medium mass flow meter 14, and the solenoid valve 13 by the auxiliary medium generation or storage unit 16, and then expands with the high temperature and high pressure fluid through the solenoid valve 17.
  • the high temperature and high pressure fluid processing area of the processing system 12 is connected.
  • the auxiliary medium used can be composed of one, two, or more than two components, and it can be a polar solvent medium, or other non-polar media such as various non-polar media. Polar solvent.
  • the circulation processing system consists of a circuit connecting the outlet of the high-temperature and high-pressure fluid puffing processing system 12 through the solenoid valve 17 and the solenoid valve 13, and then through the solenoid valve 11, the stop valve 10, the two-way fluid medium circulating pump 9, and the heat exchanger 7 in turn.
  • the medium volume flow meter 8 is connected with the high temperature and high pressure fluid puffing processing system 12, and performs high temperature and high pressure fluid processing processing on the loaded material in the high temperature and high pressure fluid processing zone under predetermined conditions.
  • the carbon dioxide separation and recovery system is the solenoid valve 18, the heat exchanger 19, and the pressure relief pump 20 connected to the fluid outlet end of the high temperature and high pressure fluid puffing processing system 12 in sequence, and then connected to the mixed medium separation unit 21, the mixed medium separation unit 21
  • the output end of the filter 23, the shut-off valve 24 or the condenser 26, and the solenoid valve 25 are sequentially connected to the carbon dioxide storage tank 1 to separate and recover the carbon dioxide medium in the high temperature and high pressure fluid expansion processing system and its pipelines.
  • the carbon dioxide separation and recovery system provided by the present invention separates and recovers the gas in the fluid puffing processing system to 1. 01 X 10 5 Pa during cooperative work, and realizes the direct opening of the system under normal pressure
  • the auxiliary medium separation and recovery system is the auxiliary medium evaporator and storage unit 16 after passing through the solenoid valve 22, and then connected to the mixed medium separation unit 21 to recover the separated auxiliary medium.
  • the high temperature and high pressure fluid puffing processing system includes high temperature and high pressure fluid processing zones 12-9 and fluid puffing buffer zones 12-11, The two zones are connected by a quick opening valve 12-10.
  • the quick opening valve is a ball valve, gate valve, or plunger valve.
  • the opening time of the valve opening from 0 to 100% is 0. 070s ⁇ 10s, after the valve is opened, It can quickly connect the high-temperature and high-pressure fluid processing zone and the fluid puffing buffer zone in less than 50 seconds.
  • the upper part of the high-temperature and high-pressure fluid treatment zone 12-9 is provided with a fluid inlet hole, which is connected to the fluid inlet 12-1 via a shut-off valve 12-2; a heating device is provided around the treatment zone, and a heating jacket 12-8 is used in this embodiment ,
  • the top is the loading port, and there is a quick opening device 12-4.
  • the processing area is equipped with a stirring mechanism.
  • This embodiment uses a magnetic stirring rotor 1 2-3 and a magnetic stirring magnetic cylinder 12-5, and a magnetic stirring magnetic cylinder 12- 5 Connect with the quick opening device 12-4 of the loading port; the quick opening device of the loading port is equipped with pressure sensor/pressure gauge interface 12-6 and temperature sensor interface 12-7, high temperature and high pressure fluid processing area 12-9 There is a fluid outlet hole at the lower end of the outlet, which is connected to the fluid outlet 12-1' through the shut-off valve 12-2'. connect.
  • the periphery of the fluid puffing buffer zone 12-11 is provided with a heating device.
  • a heating jacket 12-8' is used, and the top is provided with an inlet channel, which is connected to the quick opening valve 12-10, and the outer side of the buffer zone is at the upper end position
  • the filter 12-15 is connected, and the bottom of the filter is connected with the shut-off valve 12-16.
  • the temperature of the high temperature and high pressure fluid processing zone can reach -60 ⁇ 180 ° C or above, and the pressure can reach 0 ⁇ 30MPa or above.
  • the temperature of the fluid puffing buffer zone can reach _50. (: ⁇ 150 ° C or above, the pressure can reach 0.1MPa ⁇ 20MPa or above.
  • the multifunctional supercritical fluid processing machine for materials constructed according to the structure of FIG. 1 and FIG.
  • the valve is closed. Then turn on the quick opening structure 12-4 of the high-temperature and high-pressure fluid puffing processing system 12, and fill the high-temperature and high-pressure fluid processing area 12-9 with an appropriate amount of material to be processed; or simultaneously open the solenoid valve 13 in the auxiliary medium pressurization system, using the two-way auxiliary medium
  • the negative pressure generated by the reverse operation of the booster pump 15 cooperates with material loading.
  • the temperature sensor interface 12-7 is well connected with the corresponding sensor or meter.
  • the carbon dioxide medium pressurization system composed of volumetric flowmeter 8 etc. performs quantitative pressurization of the medium in the high-temperature and high-pressure fluid treatment zone 12-9 from the fluid inlet 12-1.
  • an auxiliary medium pressurization system composed of an auxiliary medium evaporator and storage unit 16, a two-way auxiliary medium booster pump 15, an auxiliary medium mass flow meter 14, and a solenoid valve 13 can also be used to treat high temperature and high pressure fluids.
  • Zones 12-9 perform a predetermined type and proportion of auxiliary medium pressurization. Then turn on the heating jacket 12-8 configured in the system, and heat up the high-temperature and high-pressure fluid processing zone 12-9 according to the predetermined heating conditions.
  • the reversing function of the bidirectional fluid medium circulation pump 9 can also be used to perform forward and reverse circulation processing on the fluid medium in the high temperature and high pressure fluid treatment zone 12-9.
  • the magnetic stirring cylinder 12-5 and the magnetic stirring rotor 12-3 set in the system are used to stir the material to be processed to improve the uniformity of fluid processing.
  • the operation of the two-way fluid medium circulation pump 9 is stopped. And according to the specific processing methods and requirements of the processed materials (such as puffing, or foaming or chipping, etc.), the initial temperature and pressure of the fluid puffing buffer zone 12-11 are carried out by using the heating jacket 12-8' and the shut-off valve 12-16 Condition preparation. Then, the quick-opening valve 12-10 is opened at a predetermined rate and opening, and the material processed by the high-temperature and high-pressure fluid processing zone 12-9 is processed in a predetermined manner.
  • the specific processing methods and requirements of the processed materials such as puffing, or foaming or chipping, etc.
  • the condenser 26, the solenoid valve 25, the solenoid valve 18, and the shut-off valve 12-16 are sequentially opened, and the heat exchanger 19, the pressure relief pump 20, the mixed medium separation unit 21, and the filter
  • the carbon dioxide separation and recovery system composed of the condenser 23, the condenser 26, and the carbon dioxide storage tank 1 separates and recovers the carbon dioxide medium in the high-temperature and high-pressure fluid expansion processing system 12 and its corresponding pipelines.
  • the solenoid valve 22 can be opened, and an auxiliary medium separation and recovery system composed of a mixed medium separation unit 21, an auxiliary medium evaporator, and a storage unit 16 can be used for the mixed medium separation unit 21 Auxiliary media separated in the process for recovery.
  • the high temperature high pressure conduit 12 and its respective expanded fluid medium through the processing system sufficiently separated and recovered, and which the system pressure is reduced to atmospheric pressure (1. 01 X 1 0 5 Pa )
  • the pressure relief of the pump 20 is stopped, and close Solenoid valve 18.
  • the hand hole quick opening structure 12-13 of the fluid puffing buffer area is opened, and the processed material after the fluid processing is taken out, and a fluid processing of the material under a predetermined process condition is completed.
  • the material can be processed in different ways under the predetermined conditions in the next round.
  • the technology of the present invention can also use the auxiliary medium evaporator and storage unit 16, the two-way auxiliary medium booster pump 15, the auxiliary medium mass flow meter 14, and the solenoid valve 13 as the auxiliary medium pressurization system to predict First, pressurize the auxiliary medium of a predetermined type and amount in the high-temperature and high-pressure fluid treatment zone 12-9. And use the aforementioned fluid circulation processing system to pretreat the material under different conditions, and then use the carbon dioxide medium pressurization system to pressurize the carbon dioxide medium, so as to process the material with a single supercritical carbon dioxide fluid or a mixed fluid containing auxiliary media. .

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Abstract

一种用于材料的多功能超临界流体处理机,包括设有高温高压流体处理区(12-9)和流体膨化缓冲区(12-11)的高温高压流体膨化加工系统(12)、辅助介质增压系统、二氧化碳介质增压系统、循环处理系统、二氧化碳分离回收系统、辅助介质分离回收系统。高温高压流体处理区(12-9)、流体膨化缓冲区(12-11)及其连接的快开阀(12-10),可根据工艺要求有效实现对材料不同方式如膨化、发泡、碎裂等加工处理,扩展了设备的功能多样性和应用范围;辅助介质增压系统,对材料可便捷开展任意比例混合流体介质的单独或分步膨化等加工,可实现对材料进行加工前的预处理,并对加工过程中二氧化碳流体的介质极性进行实时调控。具有适应性广,加工方式多样化、效率高、操作简便、生态环保等优点。

Description

一 种用 于材 料 的多功 能 超临 界流 体处 理机 技术领域
[0001] 本发明涉及材料的一种多功能超临界流体处理机, 属压力容器、 纺织染整加工 、 材料加工、 食品及饲料等加工设备制造技术领域。 背景技术
[0002] 材料的膨化、 发泡、 碎裂等加工处理, 在纺织、 食品、 建材、 农作物副产物加 工、 饲料、 新型材料制造、 化工、 航空航天、 医疗卫生等工农业领域中具有重 要应用。 通过材料的上述处理加工, 可以较为容易地改变材料本来的结构及体 积, 并赋予材料以多样化的功能或特性。 如在建材和新型材料制造领域可实现 材料的轻量化, 提高材料的隔热性、 形态稳定性、 应力应变特性等。 而在食品 、 农作物加工和饲料行业, 则可改善原材料的可加工性、 消化吸收特性、 利用 效率, 以及改善食品的营养特性及口味或风味等。 然而, 材料的此类传统的加 工方法通常较多采用水热法等方式, 使被处理材料或原料在含有一定水分, 其 在受热、 加压的条件下, 然后突然失压, 使材料中的水蒸气发生膨胀, 从而达 到膨化、 发泡 (或因添加的发泡剂产生气体而使材料膨胀) , 甚至碎裂等效果 。 然而, 该类传统加工方法, 对亲水性材料或含有亲水性组分的材料, 以及各 类较为疏松、 多孔天然材料等, 效果比较明显。 但对很多疏水性强、 结构致密 、 内聚能密度高的材料, 其处理效果通常有限。 且当加入发泡剂等助剂增效时 , 往往还会引入相关反应产物等杂质, 影响到材料的纯度或性能, 或给加工的 产品带来负面影响。 因而, 开发一种高效、 适用性广、 无其他副产物残留、 生 态环保的材料处理设备及其方法, 具有重要意义。
[0003] 超临界二氧化碳流体介质因其具有独特的技术特点和优势, 近年来在材料加工 领域受到广泛关注。 特别是该介质生物相容性优良、 无色无味、 不燃、 不爆、 无毒, 其生态环保特性显著。 同时, 其临界点 (31. 1°C和 7. 38MPa) 相对较低, 容易达到超临界流体状态, 其气源易得, 易于进行工业化生产加工。 更为重要 的是, 该介质的超临界流体粘度低, 扩散性、 渗透及穿透性好, 容易实现对紧 密固体材料、 疏水性材料或难穿透、 难渗透的加工材料等具有高效性。 同时也 可适用于各类亲水性材料, 以及各类无机材料的处理加工。 且可有效缩短工艺 时间, 降低成本。 在加工过程中, 无需使用和消耗水资源, 被加工物呈干态; 工艺结束后该介质也非常容易分离回收和循环使用, 在加工产品上无有害有害 物质或其他杂志残留, 加工结束后产品也无需干燥。 然而, 根据现有文献, 对 于利用超临界二氧化碳流体介质, 可实现对材料膨化、 发泡、 碎裂等加工处理 的多功能设备, 目前尚无相关报道。 发明概 述 技术问题 问题的解 决方案 技术解决方案
[0004] 本发明针对现有技术存在的不足, 提供一种具有高效、 适用性广、 操作简单、 系统稳定、 清洁环保、 无噪音影响等优点, 可有效实现对各类材料的超临界二 氧化碳流体的膨化等加工的多功能超临界流体处理机。
[0005] 为实现本发明目的所采用的技术方案是: 提供一种用于材料的多功能超临界流 体处理机, 它包括高温高压流体膨化加工系统、 二氧化碳介质增压系统、 辅助 介质增压系统、 循环处理系统、 二氧化碳分离回收系统和辅助介质分离回收系 统; 所述的高温高压流体膨化加工系统包括高温高压流体处理区和流体膨化缓 冲区, 所述的高温高压流体膨化加工系统与循环处理系统相连, 循环处理系统 一端与二氧化碳分离回收系统相连, 另一端与二氧化碳介质增压系统相连; 所 述的辅助介质增压系统一端接入循环处理系统, 另一端与二氧化碳分离回收系 统相连; 二氧化碳分离回收系统与二氧化碳介质增压系统相连通。
[0006] 本发明技术的优化方案为:
[0007] 所述的高温高压流体处理区的顶部为装料口, 设有快开结构密封盖, 高温高压 流体处理区的内部设有搅拌机构, 上部设有流体入口, 下部设有流体出口, 底 部设有出口通道; 所述的流体膨化缓冲区的顶部设有入口通道, 上部设有高压 视窗, 下部设有快开结构的手孔, 多孔网板或承接板置于流体膨化缓冲区的下 部, 底部设有出口, 通过管道依次与过滤器、 截止阀连接; 高温高压流体处理 区底部的出口通道通过快开阀与流体膨化缓冲区顶部的入口通道相连通。
[0008] 高温高压流体处理区和流体膨化缓冲区的周围分别设有加热装置; 搅拌机构包 括磁力搅拌转子和磁力搅拌磁缸, 磁力搅拌磁缸固定于快开结构密封盖上; 快 开结构密封盖上和流体膨化缓冲区的顶部, 分别设有压力表、 温度表及传感器 接口; 快开阀为球阀、 闸阀、 柱塞阀中的一种, 阀门开度从 0到 100%的开启时间 为 0. 070s〜 10s。
[0009] 本发明提供的用于材料的多功能超临界二氧化碳流体闪爆机, 所述的二氧化碳 介质增压系统包括 C0 2储罐、 质量流量计、 热交换器和增压泵; 所述的循环处理 系统包括双向流体介质循环泵、 换热器和流量计; 所述的二氧化碳分离回收系 统包括热交换器、 泄压泵、 分离单元、 过滤器、 冷凝器和二氧化碳储罐; 在工 作状态, 将流体闪爆系统内的气体分离回收至 1. 01 X 10 5Pa。
[0010] 本发明提供的一种用于材料的多功能超临界二氧化碳流体闪爆机, 其高温高压 流体处理区, 温度达到 180°C或以上, 压力达到 30MPa或以上; 其流体膨化缓冲 区, 温度达到 _50°C〜 150°C或以上, 压力达到(X IMPa〜 20MPa或以上。
[0011] 本发明提供的用于材料的多功能超临界流体闪爆机, 所适用于加工的材料, 可 以是纺织纤维材料及其制品, 以及各类合成或天然高分子有机材料, 或各类无 机材料, 也可以是各类复合材料, 还可以是食品、 饲料、 农作物副产物类材料 。 所使用的辅助介质, 可以由一种或两种, 或两种以上成分构成, 可以是极性 溶剂介质, 或其他非极性介质如各类非极性溶剂。 发明的 有益效果 有益效果
[0012] 与现有技术方案相比, 本发明具有以下显著优点:
[0013] 1.本发明提供的用于材料的多功能超临流体处理机, 由于在流体膨化加工系统 中设立了高温高压流体处理区, 并配合其循环处理系统时, 可有效实现对各类 材料的高温高压超临界流体均匀高效处理, 也有利于流体介质向材料内部扩散 和渗透, 特别是对质地紧密、 扩散阻力大的固体材料。 同时, 膨化加工系统中 设立的快开阀及流体膨化缓冲区, 可有效调控阀的开度及开启速率、 处理终态 时的温度和压力, 以分别调控并达到对材料不同工艺、 不同程度的膨化、 发泡 、 碎裂等加工处理, 从而扩展了该设备的功能多样性和应用范围。
[0014] 2.本发明在系统配置中设置了辅助介质增压系统、 二氧化碳介质增压系统、 二 氧化碳分离回收系统、 辅助介质分离回收系统, 可在高温高压流体膨化加工系 统及其循环处理系统中, 实现一种或一种以上任意比例混合流体介质的单独或 综合膨化等处理加工。 尤其是可利用辅助介质增压系统中的极性介质或非极性 介质, 不但非常容易实现对材料进行膨化等处理加工前的预处理, 而且更实现 了在高温高压处理加工过程中对二氧化碳流体介质极性进行实时调整。 特别是 利用辅助介质增压系统中的极性介质, 可显著提高对高极性材料, 如亲水性类 或含亲水性类材料的加工处理效果。
[0015] 3.本发明在辅助介质增压系统中设置的双向辅助介质增压泵, 当反向运行形成 负压, 可大大提高高温高压流体膨化加工系统中材料的装载效率。 同时, 配置 的二氧化碳分离回收系统、 辅助介质分离回收系统, 可实现对处理加工结束后 各类混合流体介质的高效分离及回收, 提高了介质的循环利用效率, 并可实现 常压直接开盖, 大大提高了设备的运行效率及经济效益。
[0016] 4.本发明提供的技术方案可实现对材料的膨化、 发泡、 碎裂等多种功能处理加 工, 并可适用于不同极性、 不同种类的有机或无机材料处理。 特别是利用超临 界二氧化碳流体介质组分的低粘度、 高渗透及穿透性强等优势, 可容易实现对 致密固体和难渗透材料的膨化等加工处理。 这对开展相关材料的绿色、 生态、 安全化加工具有重要意义, 同时也具有非常广阔的应用前景。 因而, 利用超临 界二氧化碳流体介质的这些独特优势, 将其用于各类材料的膨化、 发泡、 碎裂 等加工处理, 具有广阔的市场前景。 对附图 的简要说 明 附图说明
[0017] 图 1是本发明实施例提供的一种用于材料的多功能超临界流体处理机的系统结 构示意图;
[0018] 图 2是本发明实施例提供的高温高压流体膨化加工系统的剖面结构示意图。
[0019] 图 1中: 1、 C0 2储罐; 2 (3、 10、 24、 27) 、 截止阀; 4、 增压泵; 5、 质量 流量计; 6 (11、 13、 17、 18、 22、 25) 、 电磁阀; 7 (19) 、 热交换器; 8、 体 积流量计; 9、 双向流体介质循环泵; 12、 高温高压流体膨化加工系统; 14、 辅 助介质质量流量计; 15、 双向辅助介质增压泵; 16、 辅助介质蒸发器及储存单 元; 20、 泄压泵; 21、 混合介质分离单元; 23、 过滤器; 26、 冷凝器; 28、 C0 2 气体入口。
[0020] 图 2中: 12-1、 流体入口; 12-1’、 流体出口; 12-2 ( 12-2’、 12-16) 、 截止阀 ; 12-3、 磁力搅拌转子; 12-4、 快开结构; 12-5、 磁力搅拌磁缸; 12-6、 压力 传感器 /压力表接口; 12-7、 温度传感器接口; 12-8 ( 12-8’ ) 、 加热套; 12-9 、 高温高压流体处理区; 12-10、 快开阀; 12-11、 流体膨化缓冲区; 12-12、 高 压视窗; 12-13、 膨化加工区手孔快开结构; 12-14、 多孔网板或承接板; 12-15 、 过滤器。 发明实施 例 本发明的实施方 式
[0021] [0008] 下面结合附图和实施例对本发明技术方案作进一步描述。
[0022] 实施例 1
[0023] 本实施例提供一种用于材料的多功能超临界流体处理机, 所加工的适用材料, 可以是纺织纤维材料及其制品, 以及各类合成或天然高分子有机材料, 或各类 无机材料, 也可以是各类复合材料, 还可以是食品、 饲料、 农作物副产物类材 料。
[0024] 参见附图 1, 它是本实施例提供的用于材料的多功能超临界流体处理机的系统 结构示意图; 它包括高温高压流体膨化加工系统、 二氧化碳介质增压系统、 辅 助介质增压系统、 循环处理系统、 二氧化碳分离回收系统和辅助介质分离回收 系统。 具体结构如下:
[0025] 二氧化碳介质增压系统由 C0 2气体入口 28设截止阀 27与 C0 2储罐 1连通, C0 2 储罐 1的底部出口设截止阀 2, C0 2储罐 1的出口端经截止阀 3, 依次连接增压泵 4 、 质量流量计 5、 电磁阀 6、 热交换器 7, 再经体积流量计 8, 与高温高压流体膨 化加工系统 12的流体进口端连通。
[0026] 辅助介质增压系统由辅助介质发生或储存单元 16依次连接双向辅助介质增压泵 15、 辅助介质质量流量计 14、 电磁阀 13, 再通过电磁阀 17与高温高压流体膨化 加工系统 12的高温高压流体处理区连通。 本发明提供的多功能超临界流体处理 机, 所使用的辅助介质, 可以由一种或两种, 或两种以上成分构成, 可以是极 性溶剂介质, 或其他非极性介质如各类非极性溶剂。
[0027] 循环处理系统由高温高压流体膨化加工系统 12的出口经电磁阀 17和电磁阀 13连 接的回路, 再依次经电磁阀 11、 截止阀 10、 双向流体介质循环泵 9、 换热器 7、 介质体积流量计 8, 与高温高压流体膨化加工系统 12连通, 对高温高压流体处理 区中的装载材料进行预定条件的高温高压流体处理加工。
[0028] 二氧化碳分离回收系统为高温高压流体膨化加工系统 12的流体出口端依次连接 的电磁阀 18、 热交换器 19、 泄压泵 20后, 再连接混合介质分离单元 21, 混合介 质分离单元 21的输出端经依次连接过滤器 23、 截止阀 24或冷凝器 26、 电磁阀 25 , 连通二氧化碳储罐 1, 对高温高压流体膨化加工系统及其管路中的二氧化碳介 质进行分离和回收。 本发明所提供的二氧化碳分离回收系统, 在协同工作时将 流体膨化加工系统内的气体分离回收至 1. 01 X 10 5Pa, 实现系统的常压直接开盖
[0029] 辅助介质分离回收系统为辅助介质蒸发器及储存单元 16经电磁阀 22后, 再连接 混合介质分离单元 21, 对分离的辅助介质进行回收。
[0030] 参见附图 2, 它是本实施例提供的高温高压流体膨化加工系统剖面结构示意图 ; 高温高压流体膨化加工系统包括高温高压流体处理区 12-9和流体膨化缓冲区 1 2-11, 两个区通过快开阀 12-10相连, 快开阀为球阀、 闸阀、 柱塞阀中的一种, 阀门开度从 0到 100%的开启时间为 0. 070s〜 10s, 阀门开启后, 能在小于 50秒的 时间内快速连通高温高压流体处理区及流体膨化缓冲区。
[0031] 高温高压流体处理区 12-9上部开有流体入口孔, 经截止阀 12-2与流体入口 12-1 连通; 处理区周围设有加热装置, 本实施例中采用加热套 12-8, 顶部为装料口 , 设有快开装置 12-4, 处理区内部设有搅拌机构, 本实施例采用磁力搅拌转子 1 2-3和磁力搅拌磁缸 12-5, 磁力搅拌磁缸 12-5与装料口的快开装置 12-4相连接; 装料口的快开装置上设有压力传感器 /压力表接口 12-6和温度传感器接口 12-7, 高温高压流体处理区 12-9下端出口处开有流体出口孔, 经截止阀 12-2’与流体出 口 12-1’连通, 高温高压流体处理区 12-9的底部设有出口通道, 与快开阀 12-10 连接。
[0032] 流体膨化缓冲区 12-11的外围设有加热装置, 本实施例中采用加热套 12-8’, 顶 部设有入口通道, 与快开阀 12-10相连, 缓冲区外侧靠上端位置处设有对称的高 压视窗 12-12, 下端靠底部位置设有快开结构的手孔 12-13, 底部设有多孔网板 或承接板 12-14; 流体膨化缓冲区的底部出口处与过滤器 12-15相连, 过滤器下 方与截止阀 12- 16连接。
[0033] 利用本发明提供的多功能超临界流体处理机, 高温高压流体处理区的温度可达 -60〜 180°C或以上, 压力可达 0〜 30MPa或以上。 流体膨化缓冲区的温度可达 _50 。(:〜 150°C或以上, 压力可达 0. IMPa〜 20MPa或以上。
[0034] 依据本发明工作原理, 利用按图 1和图 2结构构建的用于材料的多功能超临界流 体处理机, 在准备开启工作模式时, 先将各系统及单元、 管线上的各类阀门处 于关闭状态。 然后开启高温高压流体膨化加工系统 12的快开结构 12-4, 向高温 高压流体处理区 12-9装填适量待处理材料; 或同时开启辅助介质增压系统中的 电磁阀 13, 利用双向辅助介质增压泵 15反向运行产生的负压, 协同进行材料装 载。 装填完成后, 关闭高温高压流体膨化加工系统 12中的快开结构 12-4, 并按 序组装好磁力搅拌转子 12-3、 磁力搅拌磁缸 12-5, 使压力传感器 /压力表接口 12 -6、 温度传感器接口 12-7与对应传感器或仪表连接良好。 然后打开截止阀 12-2 和截止阀 3、 电磁阀 6, 开启增压泵 4, 并根据处理工艺要求, 利用由二氧化碳储 罐 1、 增压泵 4、 质量流量计 5、 热交换器 7、 体积流量计 8等组成的二氧化碳介质 增压系统, 从流体入口 12-1对高温高压流体处理区 12-9进行介质的定量增压。 同时, 根据具体工艺要求, 还可以由辅助介质蒸发器及储存单元 16、 双向辅助 介质增压泵 15、 辅助介质质量流量计 14、 电磁阀 13组成的辅助介质增压系统, 对高温高压流体处理区 12-9进行预定种类及比例的辅助介质增压。 然后开启系 统配置的加热套 12-8, 按预定升温条件对高温高压流体处理区 12-9进行加热升
[0035] 流体介质增压结束后, 关闭增压泵 4、 电磁阀 6, 并开启截止阀 12-2’、 电磁阀 1 7、 电磁阀 11、 双向流体介质循环泵 9, 利用由高温高压流体膨化加工系统 12中 高温高压流体处理区 12-9、 流体出口 12-1’、 电动阀 17和电动阀 13连接的回路、 双向流体介质循环泵 9、 热交换器 7、 体积流量计 8等组成的循环处理系统, 对高 温高压流体处理区 12-9中的装载材料进行预定条件的高温高压流体处理加工。 同时, 也可以根据加工要求, 采用双向流体介质循环泵 9的换向功能, 对高温高 压流体处理区 12-9中的流体介质进行正反向循环处理。 并采用系统设置的磁力 搅拌磁缸 12-5和磁力搅拌转子 12-3对被处理材料进行搅拌, 提高其流体处理的 均匀性。
[0036] 当高温高压处理工艺段结束后, 停止双向流体介质循环泵 9的运行。 并根据对 处理材料的具体加工方式及要求 (如膨化, 或发泡或碎裂等) , 利用加热套 12- 8’、 截止阀 12-16对流体膨化缓冲区 12-11进行初始温度和压力条件准备。 然后 按预定速率和开度开启快开阀 12-10, 对经过高温高压流体处理区 12-9处理的材 料进行预定方式加工处理。 此外, 在进行流体膨化等处理加工过程中, 还可以 借助流体膨化缓冲区 12-11设置的高压视窗 12-12, 对材料的流体加工全过程进 行在线观察及记录, 可为研究不同流体及其加工条件等对不同材料、 不同处理 方式的加工过程及机理等提供条件。
[0037] 材料的流体加工处理结束后, 依次开启冷凝器 26、 电磁阀 25、 电磁阀 18、 截止 阀 12-16, 利用由热交换器 19、 泄压泵 20、 混合介质分离单元 21、 过滤器 23、 冷 凝器 26、 二氧化碳储罐 1等组成的二氧化碳分离回收系统, 对高温高压流体膨化 加工系统 12及其相应管路中的二氧化碳介质进行分离和回收。 同时, 在二氧化 碳介质分离回收过程中或其完成后, 可开启电磁阀 22, 采用由混合介质分离单 元 21、 辅助介质蒸发器及储存单元 16组成的辅助介质分离回收系统, 对混合介 质分离单元 21中分离的辅助介质进行回收。 当高温高压流体膨化加工系统 12及 其相应管路中的介质经充分分离回收后, 且其系统压力降低至大气压 ( 1. 01 X 1 0 5Pa) 时, 泄压泵 20停止工作, 并关闭电磁阀 18。 然后打开流体膨化缓冲区手 孔快开结构 12-13, 取出经流体加工处理后的被处理材料, 完成一次预定工艺条 件下的材料流体加工处理。
[0038] 重复上述操作, 可实现下一轮预定条件下材料的不同方式加工处理。
[0039] 本发明技术根据需要, 还可以利用辅助介质蒸发器及储存单元 16、 双向辅助介 质增压泵 15、 辅助介质质量流量计 14、 电磁阀 13组成的辅助介质增压系统, 预 先对高温高压流体处理区 12-9进行预定种类及用量的辅助介质增压。 并利用前 述流体循环处理系统对材料进行不同条件的预处理, 然后再利用二氧化碳介质 增压系统进行二氧化碳介质的增压, 从而对材料进行单独的超临界二氧化碳流 体或含辅助介质的混合流体加工处理。

Claims

权利 要 求 书
[权利要求 1] 一种用于材料的多功能超临界流体处理机, 其特征在于: 它包括高温 高压流体膨化加工系统、 二氧化碳介质增压系统、 辅助介质增压系统 、 循环处理系统、 二氧化碳分离回收系统和辅助介质分离回收系统; 所述的高温高压流体膨化加工系统包括高温高压流体处理区和流体膨 化缓冲区, 通过快开阀相连通; 所述的高温高压流体膨化加工系统与 循环处理系统相连, 循环处理系统一端与二氧化碳分离回收系统相连 , 另一端与二氧化碳介质增压系统相连; 所述的辅助介质增压系统一 端接入循环处理系统, 另一端与二氧化碳分离回收系统相连; 二氧化 碳分离回收系统与二氧化碳介质增压系统相连通。
[权利要求 2] 根据权利要求 1所述的一种用于材料的多功能超临界流体处理机, 其 特征在于: 所述的高温高压流体处理区的顶部为装料口, 设有快开结 构密封盖, 高温高压流体处理区的内部设有搅拌机构, 上部设有流体 入口, 下部设有流体出口, 底部设有出口通道; 所述的流体膨化缓冲 区的顶部设有入口通道, 上部设有高压视窗, 下部设有快开结构的手 孔, 多孔网板或承接板置于流体膨化缓冲区的下部, 底部设有出口, 通过管道依次与过滤器、 截止阀连接; 高温高压流体处理区底部的出 口通道通过快开阀与流体膨化缓冲区顶部的入口通道相连通。
[权利要求 3] 根据权利要求 1所述的一种用于材料的多功能超临界流体处理机, 其 特征在于: 所述的二氧化碳介质增压系统包括 C0 2储罐、 质量流量计 、 热交换器和增压泵。
[权利要求 4] 根据权利要求 1所述的一种用于材料的多功能超临界流体处理机, 其 特征在于: 所述的循环处理系统包括双向流体介质循环泵、 换热器和 流量计。
[权利要求 5] 根据权利要求 1所述的一种用于材料的多功能超临界流体处理机, 其 特征在于: 所述的二氧化碳分离回收系统包括热交换器、 泄压泵、 分 离单元、 过滤器、 冷凝器和二氧化碳储罐; 在工作状态, 将流体闪爆 系统内的气体分离回收至 1. 01 X 10 5Pa。 [权利要求 6] 根据权利要求 1或 2所述的一种用于材料的多功能超临界流体处理机, 其特征在于: 高温高压流体处理区和流体膨化缓冲区的周围分别设有 加热装置。
[权利要求 7] 根据权利要求 1或 2所述的一种用于材料的多功能超临界流体处理机, 其特征在于: 所述的快开阀为球阀、 闸阀、 柱塞阀中的一种, 阀门开 度从 0到 100%的开启时间为 0. 070s〜 10s。
[权利要求 8] 根据权利要求 1或 2所述的一种用于材料的多功能超临界流体处理机, 其特征在于: 所述的高温高压流体处理区, 温度达到 180°C或以上, 压力达到 30MPa或以上; 所述的流体膨化缓冲区, 温度达到 -50°C〜 15 0°C或以上, 压力达到 0. IMPa〜 20MPa或以上。
[权利要求 9] 根据权利要求 2所述的一种用于材料的多功能超临界流体处理机, 其 特征在于: 所述的搅拌机构包括磁力搅拌转子和磁力搅拌磁缸, 磁力 搅拌磁缸固定于快开结构密封盖上。
[权利要求 10] 根据权利要求 2所述的一种用于材料的多功能超临界流体处理机, 其 特征在于: 快开结构密封盖上和流体膨化缓冲区的顶部, 分别设有压 力表、 温度表及传感器接口。
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