SFED-25超临界干燥装置

一、概述
    超临界干燥技术是近年来发展起来的化工新技术。由于凝胶骨架内部的溶剂存在表面张力，在普通的干燥条件下会造成骨架的坍缩。超临界干燥旨在通过压力和温度的控制，使溶剂在干燥过程中达到其本身的临界点，完成液相至超临界流体转变。过程中溶剂无明显表面张力，在维持骨架结构的前提下完成湿凝胶向气凝胶的转变。
    超临界干燥的基本原理是：在超临界状态下，气体和液体之间不再有界面存在，而是成为介于气体和液体之间的一种均匀的流体。这种流体逐渐从凝胶中排出，由于不存在气-液界面，也就不存在毛细管力，因此不会引起凝胶体的收缩和结构的破坏，直至全部流体都从凝胶中排出，得到充满气体的，具有纳米孔结构的材料
二、装置特点
2-1、装置操作人性化设计，面板设计流程，可根据流程操作阀门。
2-2、干燥釜、采用自行研制的快开密封结构，打开非常轻松，密封相当可靠，遇CO2不溶胀且重复性好，有效地解决了O形圈遇CO2膨胀的难题。
2-3、采用PID程序控温技术，干燥釜内温度均匀，控温精度高。
2-4、制冷机组采用进口压缩机，运行稳定，其它制冷配件均选用国际知名品牌产品。
2-5、CO2泵使用三柱塞泵头，降低流体压力波动。泵头带冷却系统，柱塞采用特殊耐磨材料制造。
2-6、压力控制系统，采用美国进口阀门，具有压力调节精度高，出口压力平稳，输出流量大等优点。
2-7、安全辅助系统包括单向阀门和安全阀、放空阀等硬性安全保护措施，以及电接点仪表，报警自断电路等软性安全保护措施。保证系统高压环境下的安全稳定工作。    
三、主要技术参数
    干燥釜：25L/30MPa      室温～90℃
    分离釜：10L/15MPa      室温～60℃
    制冷系统：9600kcal/h   风冷水循环
    储罐：10L/16MPa
    CO2高压输送泵：三柱塞    150L/40MPa    泵头带冷却
    电源：三相五线制380V/50Hz    整机功率28kW
四、主要组成部件
    超临界干燥装置主要由：CO2气源系统、制冷系统、热交换器系统、温度控制系统、压力控制系统、干燥釜、分离釜及电气控制、过滤器净化器系统、CO2利用循环回收系统、支架箱体等组成。
五、各主要部件技术指标
5-1、气源系统：
    一般采用CO2为干燥介质该系统为用户自备，若非国内气瓶供应或非气瓶直接供应，则需提供气源接入口规格尺寸，以便本装置接入系统正常运行。
5-2、制冷系统：
    制冷系统将二氧化碳气体液化，为系统高压注入的稳定、可靠提供保障。制冷机组采用进口压缩机，运行稳定，其它制冷配件均选用国际知名品牌产品。根据试验条件，控制系统自动调节制冷机运行工况、冷量大小，确保压缩机工作在合适状态，延长压缩机使用寿命。环保制冷剂R404a；制冷机专用减振弹簧、机组围板粘贴特种吸音棉降噪措施。具体技术指标如下：
    制冷量：9600kcal/h
    制冷方式：风冷水循环
    温控范围：3℃～+5℃满足工艺要求
5-3、高压输送泵：
    作为系统高压注入的主要部件，CO2高压计量泵主要由电机、变频调速控制系统、变速机构、安全阀和液缸体等组成。电机动力通过变速机构由凸轮带动弓架及滑杆作往复运动。柱塞安装在滑杆顶端，连动柱塞往复，通过单向阀的作用，完成吸排过程，排量由频率调速控制，以控制流量大小。泵头带冷却系统，柱塞采用特殊耐磨材料制造，使用三柱塞，降低流体波动。主要技术指标：
    工作压力：40MPa  
    排量：150L/h    三柱塞
5-4、流量计量系统：
    采用气体质量流量计结合流量数显仪表对管路中的CO2气体进行计量，流量控制范围：15～150L/h
5-5、温度控制系统：
    采用PID程序升温控温与水浴配合换热，提高换热稳定性，在使用过程中，根据升温幅度进行调节。设定温度梯度调节数值，系统进行自整定自动控制，整个过程自动完成，无需人工操作。
    温度控制范围：常温～90℃
5-6、压力控制系统：
    入口压力：≤32MPa，出口压力：0～32MPa，适用介质：弱腐蚀性
5-7、凝胶干燥釜：
    容积25L，内部精密打磨处理，设计压力30MPa，温度90℃，内部带有测温，外部设计保温隔热装置。干燥器的长径比根据凝胶样品制作的特殊性进行单独设计。
    为提高干燥装置的适用范围，满足不同干燥介质进行样品处理的要求，干燥器设计温度和压力均比较高，可在很大范围内对样品制作条件进行调节。
5-8、分离装置：
    分离装置是气液分离的主要场所，大部分液体在此得到有效回收，回收液收集后可再度循环利用，气体则通过上部的出口进入下一环节。
    分离容积：10L
    分离压力：15MPa
5-9、热交换器：
    供热系统包括热箱及热力循环泵，其中预热管工作压力为50MPa，操作温度90℃，热力循环泵采用耐腐耐温的管道泵，具有耐热、耐腐、耐用、噪音小等特点。
5-10、安全保护装置：
5-10-1、高压泵出口配电接点压力表、设定工作压力、超压自动停泵保护。
5-10-2、干燥釜、分离釜、根据工作压力，分别配安全阀，超压自动泄压。
5-11、管路、阀门配件：
    接触流体的容器、阀门、管件、管线均采用DW8系列316L不锈钢材质。阀门的阀杆经特殊热处理，坚久耐用。
5-12、电气控制及箱体支架：
    根据现代实验室要求进行设备的外形设计，美观大方。采用工业铝型材主体结构，人机操作环境，布置得体，与现代实验室搭配和谐。

I. Overview

Supercritical drying technology is a new chemical technology developed in recent years. Because of the surface tension of the solvent in the gel skeleton, the skeleton will collapse under ordinary drying conditions. Supercritical drying aims to make the solvent reach its critical point during the drying process by controlling the pressure and temperature, and complete the transition from liquid phase to supercritical fluid. In the process, the solvent has no obvious surface tension, and the transformation from wet gel to aerogel is completed on the premise of maintaining the skeleton structure.

The basic principle of supercritical drying is that there is no interface between gas and liquid in supercritical state, but it becomes a uniform fluid between gas and liquid. This fluid is gradually discharged from the gel. Because there is no gas-liquid interface, there is no capillary force, so it will not cause the contraction of the gel and the destruction of the structure until all the fluid is discharged from the gel, and the gas-filled material with nano-porous structure is obtained.

Second, the device characteristics

2-1. User-friendly design of device operation, panel design process, and valve operation according to the process.

2-2. The drying kettle adopts a self-developed quick-opening sealing structure, which is very easy to open, reliable in sealing, does not swell in case of CO2 and has good repeatability, effectively solving the problem of O-ring swelling in case of CO2.

2-3. Using PID program temperature control technology, the temperature in the drying kettle is uniform and the temperature control accuracy is high.

2-4. The refrigeration unit adopts imported compressor, which runs stably. Other refrigeration accessories are internationally renowned brand products.

2-5. The CO2 pump uses three plunger pump heads to reduce fluid pressure fluctuation. The pump head is equipped with a cooling system, and the plunger is made of special wear-resistant materials.

2-6. The pressure control system adopts American imported valves, which has the advantages of high pressure adjustment accuracy, stable outlet pressure and large output flow.

2-7. Safety auxiliary system includes hard safety protection measures such as one-way valve, safety valve and vent valve, and soft safety protection measures such as electric contact instrument and alarm self-breaking circuit. Ensure the safe and stable operation of the system under high pressure environment.     

III. Main technical parameters

Drying kettle: 25L/30MPa at room temperature ~ 90℃

Separation kettle: 10L/15MPa at room temperature ~ 60℃

Refrigeration system: 9600kcal/h air-cooling water circulation.

Storage tank: 10L/16MPa

CO2 high-pressure delivery pump: three-plunger 150L/40MPa pump with cooling head.

Power supply: three-phase five-wire system 380V/50Hz, and the overall power is 28kW.

Four, the main components

The supercritical drying device is mainly composed of CO2 gas source system, refrigeration system, heat exchanger system, temperature control system, pressure control system, drying kettle, separation kettle and electrical control, filter purifier system, CO2 utilization and recycling system, and bracket box.

Five, the main components of technical indicators

5-1. Air supply system:

Generally, CO2 is used as the drying medium. This system is provided by the user. If it is not supplied by domestic gas cylinders or directly by non-gas cylinders, the specification and size of the gas source access port shall be provided for the normal operation of the device access system.

5-2, refrigeration system:

The refrigeration system liquefies carbon dioxide gas, which ensures the stability and reliability of high-pressure injection in the system. The refrigeration unit adopts imported compressor, which runs stably, and other refrigeration accessories are internationally renowned brand products. According to the test conditions, the control system automatically adjusts the operating conditions and cooling capacity of the refrigerator to ensure the compressor to work in a suitable state and prolong the service life of the compressor. Environmental protection refrigerant R404a；; Special damping spring for refrigerator and noise reduction measures by sticking special sound-absorbing cotton on the enclosure board of the unit. Specific technical indicators are as follows:

Refrigeration capacity: 9600kcal/h

Refrigeration mode: air-cooling water circulation

Temperature control range: 3℃ ~+5℃ meets the process requirements.

5-3, high pressure pump:

As the main component of high-pressure injection system, CO2 high-pressure metering pump is mainly composed of motor, variable frequency speed control system, speed change mechanism, safety valve and hydraulic cylinder. The motor power drives the bow frame and the sliding bar to reciprocate through the speed change mechanism by the cam. The plunger is installed at the top end of the slide bar, and the plunger is linked to reciprocate. Through the action of one-way valve, the suction and discharge process is completed, and the displacement is controlled by frequency speed regulation to control the flow. The pump is equipped with cooling system, and the plunger is made of special wear-resistant material, using three plungers to reduce fluid fluctuation. Main technical indicators:

Working pressure: 40MPa

Displacement: 150L/h three plungers.

5-4. Flow metering system:

The CO2 gas in the pipeline is measured by gas mass flowmeter combined with flow digital display instrument, and the flow control range is 15 ~ 150 L/h.

5-5, temperature control system:

PID programmed temperature control and water bath are used to improve the heat transfer stability, and the temperature is adjusted according to the temperature rise range during use. Setting the temperature gradient adjustment value, the system carries out self-tuning automatic control, and the whole process is completed automatically without manual operation.

Temperature control range: normal temperature ~ 90℃

5-6, pressure control system:

Inlet pressure: ≤32MPa, outlet pressure: 0 ~ 32mpa, and applicable medium: weakly corrosive.

5-7. Gel drying kettle:

The volume is 25L, the internal precision grinding treatment, the design pressure is 30MPa, the temperature is 90℃, the internal temperature is measured, and the external thermal insulation device is designed. The length-diameter ratio of the dryer is designed separately according to the particularity of gel sample making.

In order to improve the application scope of the drying device and meet the requirements of sample treatment with different drying media, the design temperature and pressure of the dryer are relatively high, and the sample preparation conditions can be adjusted in a wide range.

5-8, separation device:

The separation device is the main place for gas-liquid separation, where most of the liquid is effectively recovered, and the recovered liquid can be recycled again after collection, and the gas enters the next link through the upper outlet.

Separation volume: 10L

Separation pressure: 15MPa

5-9, heat exchanger:

The heating system includes a hot box and a thermal circulating pump, in which the working pressure of the preheating pipe is 50MPa and the operating temperature is 90℃. The thermal circulating pump adopts a pipeline pump with corrosion resistance and temperature resistance, which has the characteristics of heat resistance, corrosion resistance, durability and low noise.

5-10, safety protection device:

5-10-1, high-pressure pump outlet distribution contact pressure gauge, set working pressure, overpressure automatic pump stop protection.

5-10-2. According to the working pressure, the drying kettle and the separating kettle are respectively equipped with safety valves, which can automatically release the pressure in case of overpressure.

5-11. Piping and valve fittings:

The containers, valves, pipe fittings and pipelines in contact with fluids are made of DW8 series 316L stainless steel. The stem of the valve is durable after special heat treatment.

5-12, electrical control and box bracket:

According to the requirements of modern laboratory, the shape design of the equipment is beautiful and generous. The main structure of industrial aluminum profile is adopted, the man-machine operation environment is appropriate, and it is in harmony with modern laboratories.

南通立凯机电工程有限公司专业设计、制造、销售超临界流体设备和石油科研仪器。产品主要包括：
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