HFY-2超临界可视合成装置

一、概述：
    超临界流体具有独特的性质，如密度溶解能力接近液体，扩散系数和粘度接近气体，作为萃取溶剂广泛应用于天然产物、医药、化妆品、食品等领域，用于萃取天然活性物质、药品化妆品中活性成分、各类挥发油、香精、天然色素等，目前超临界二氧化碳萃取已经广泛应用，随着应用的不断扩展，发现超临界流体也可以用于化学反应。
    超临界流体中的化学反应可分为两大类，即超临界流体作为反应介质的反应和超临界流体作为反应原料，其中酶催化反应、超临界水氧化、金属有机反应、高分子合成等反应属于以超临界流体为反应介质的反应，应用较多，以超临界流体作为反应原料的反应有超临界二氧化碳的加氢反应，在此反应条件下，二氧化碳CO2即使反应物也是溶剂，利用二氧化碳对氢气具有非常高溶解度的特点。
    HFY超临界流体反应装置是在超临界状态下进行反应，可以提高转化率和产率，以小的反应器获得较多数量的产品。是属于连续反应，可用的反应器有：带搅拌的高温高压反应釜、带磁力搅拌反应釜、催化反应釜、固定床管式反应器等。
二、主要参数：
    合成反应釜：0.5L/15MPa  室温～150℃
    介质注入泵：0.01～9.99ml/min  精度0.01ml  40MPa
    可视反应釜：0.5L/10MPa  室温～85℃
    恒温箱：室温～150℃  600×450×550mm
    节能换热器：压力≤15MPa
    过滤收集器：3L/30MPa  材质316L
    低温冷水机：4470Kcal/h  带循环 制冷温度-10℃～常温
    电源：AC380V/50Hz  三相五线  28kW；
三、装置组成：
    装置主要由流体注入系统、换热系统、反应釜系统、控压阀、温度控制系统、压力控制系统、管阀件、安全系统、机箱支架等部分组成。
四、主要技术指标：
4-1、注入系统：
    注入系统包括介质容器、介质注入泵以及对应的管路阀门。
介质容器：
    介质容器容积1L，压力15MPa，使用温度为常温，材质为304。容器内壁精密打磨。
    溶液装入后，通过氮气管路，缓慢通入氮气对容器内空间杂气进行吹扫保护，杂气通过容器放空阀排出，驱除杂气后，关闭放空阀。
    使用结束后，需对容器内部进行清洗，并注入纯水对管路各部件进行清洗，氮气吹扫。
介质注入泵：
    型号：LB1040平流泵，采用89C52单片机与外围接口芯片组成一个微机处理系统，利用高速数据处理和定时/计数功能，通过程序控制，实现对步进电机的调速和运行状态的控制，并实时记录恒压环境下的流量曲线或恒流环境下的压力曲线。该系列泵可与计算机通讯接口，可多机通讯。
    非圆齿轮曲柄连杆机构，保证流量计量精度，耐压及平稳性好；整体式机电合一，机械传动及正题结构合理有减震防噪措施，噪音极小；具有压力测量和过压保护、欠压补偿系统；压缩自动补偿程序控制，使泵在高压工作时流量精度保持稳定。
    泵的精度较高，在泵入口端增设专用过滤器，防止细微坚硬颗粒损伤柱塞，影响正常使用。其主要技术指标如下：
    流量范围:0.01-9.99ml/min
    工作压力:0～40MPa
    重复精度％:±1
    流量精度％ :±3
管路阀门：
    泵与容器连接段管线阀门以及锥度密封件，选用φ8规格系列件，耐压50MPa，316L材质，保证该段工艺管路常温环境下的耐腐性能。
4-2、换热系统：
    换热系统包括介质预热器、恒温箱及对应管路阀门部件。
介质预热器：
    介质预热器采用盘管水浴循环换热方式，介质盘管采用φ8×2mm管线盘绕而成，管线10米，换热面积0.25M2，材质316。
    水浴加热器浴槽8L，加热功率1.2kW，热循环泵120W，材质304不锈钢，加热温度室温～100℃，温度通过控制面板仪表进行调整控制。水浴槽配备活动式液位控制器，水浴槽液位低于保护液位时，会触发保护，停止加热，防止损伤加热部件，在设备使用前，请预先检查水浴槽水位情况。
恒温箱：
    前开门，内装射灯，不锈钢内胆，采用静音轴流风机进行箱内热风循环，外部采用A3磷化喷塑，美观大气。配备脚轮和支撑脚，移动方便，定位水平可调。
    采用PID调节控温技术，箱内温度均匀，控温精度高：
    工作温度：150℃±1℃
    内胆尺寸：600×450×550㎜（长×宽×高）
管线阀门：
    该段管线阀门以及锥度密封件，选用DW8，耐压50MPa系列部件，材质根据流体和温度的不同进行对应选用。
    介质预热器入口前端部件的材质为316L；其余管路采用316管线及管接件；
4-3、背压阀：
    用于控制反应器内部的反应压力，采用高精度控压阀，控制压力0-16MPa,控制精度：0.1MPa,主体材质为316L不锈钢。
4-4、温度控制系统：
    主要用于反应釜、恒温箱温度的控制，并对主要部件温度进行采集，由温度传感器、温度数显二次仪表等组成。
    温度传感器选用PT100型温度传感器，测量范围0-200℃，输出信号：4-20mA.
    数显二次仪表：主要用于显示温度值，便于后部计算用；采用国产高精度温度数显二次表,  该类数显二次表具有较高的采集速度、较高的准确度等优点,自带RS485通讯，可实现与计算机进行通讯；
4-5、压力测量及显示：
    压力控制主要显示反应釜的压力，由压力传感器、压力控制仪两部分组成。
    压力传感器采用瑞士进口压力传感器，量程25MPa，精度可达到0.1%F.S，供电9~36V，输出4-20mA。该传感器具有较高的精度及长期的稳定性。
    压力控制仪表采用数显二次仪表，可实现与计算机的通讯；该类数显二次表具有较高的采集速度、较高的准确度等优点,自带RS485通讯，可实现与计算机进行通讯。
4-6、安全保护系统：
    设备各罐体、反应釜均配有压力表、安全阀，达到保护压力，自动泄压。
    水浴换热设置有水位保护措施，主反应器设置有压力保护措施，触动安全保护，蜂鸣提醒并自动切断相应的动力，自行阻止内部环境的增高，手动解决问题后，恢复正常。
4-7、管阀件系统：
    主要由三通、四通、管线、锥形密封件等组成，规格：Ф6-8／50MPa 316、316L材质；管路流程的连接结构紧凑，管线折弯美观大方，拆卸方便。
4-8、电气控制系统
    主要包含品牌电气元件、控制器以及散热装置、强弱电线缆以及控制系统用屏蔽线缆等。动力接线采用三相五线制，安全性高。
4-9、箱体支架：
    主要用于安装固定系统中各部件与保护装置，主体框架采用工业铝型材加工而成，高温安全保护及面板显示部分均采用不锈钢激光加工而成。

I. Overview:

Supercritical fluid has unique properties, such as density solubility close to liquid, diffusion coefficient and viscosity close to gas. As an extraction solvent, it is widely used in natural products, medicine, cosmetics, food and other fields, and is used to extract natural active substances, active ingredients in medicines and cosmetics, various volatile oils, flavors, natural pigments, etc. At present, supercritical carbon dioxide extraction has been widely used. With the continuous expansion of applications, it is found that supercritical fluid can also be used in chemical reactions.

Chemical reactions in supercritical fluid can be divided into two categories, namely, reactions with supercritical fluid as reaction medium and reactions with supercritical fluid as reaction raw material. Among them, enzyme-catalyzed reactions, supercritical water oxidation, metal-organic reactions, polymer synthesis and other reactions with supercritical fluid as reaction medium are widely used, and reactions with supercritical fluid as reaction raw material include hydrogenation of supercritical carbon dioxide. Under this reaction condition, carbon dioxide CO2 is a solvent even if it is a reactant, and carbon dioxide has a very high solubility for hydrogen.

The HFY supercritical fluid reaction device reacts in supercritical state, which can improve the conversion rate and yield, and obtain more products with a small reactor. It is a continuous reaction, and the available reactors are: high temperature and high pressure reactor with stirring, reactor with magnetic stirring, catalytic reactor, fixed bed tubular reactor, etc.

Second, the main parameters:

Synthesis reactor: 0.5L/15MPa room temperature ~ 150℃

Medium injection pump: 0.01 ~ 9.99 ml/min accuracy 0.01ml 40MPa.

Visual reactor: 0.5L/10MPa room temperature ~ 85℃

Thermobox: room temperature ~ 150℃ 600× 450× 550 mm

Energy-saving heat exchanger: pressure ≤15MPa

Filter collector: 3L/30MPa material 316L.

Low temperature water chiller: 4470Kcal/h with circulating refrigeration temperature-10℃ ~ normal temperature.

Power supply: AC380V/50Hz tn-s 28kW；;

Third, the device composition:

The device mainly consists of a fluid injection system, a heat exchange system, a reaction kettle system, a pressure control valve, a temperature control system, a pressure control system, a pipe valve, a safety system, a chassis bracket and the like.

Four, the main technical indicators:

4-1, injection system:

The injection system includes a medium container, a medium injection pump and corresponding pipeline valves.

Media container:

The volume of the medium container is 1L, the pressure is 15MPa, the service temperature is normal temperature, and the material is 304. The inner wall of the container is precisely polished.

After the solution is filled, nitrogen is slowly introduced through the nitrogen pipeline to purge and protect the miscellaneous gas in the container space, and the miscellaneous gas is discharged through the container vent valve, and the vent valve is closed after the miscellaneous gas is expelled.

After use, it is necessary to clean the inside of the container, inject pure water to clean all parts of the pipeline, and purge with nitrogen.

Medium injection pump:

Model: LB1040 advection pump. A microcomputer processing system is composed of 89C52 single chip microcomputer and peripheral interface chip. By using high-speed data processing and timing/counting functions, the speed regulation and running state of stepping motor are controlled through program control, and the flow curve under constant pressure environment or the pressure curve under constant current environment is recorded in real time. This series of pumps can communicate with computers and multiple computers.

Non-circular gear crank-connecting rod mechanism ensures flow metering accuracy, good pressure resistance and stability; Integral mechatronics, reasonable mechanical transmission and topic structure, shock absorption and noise prevention measures, and minimal noise; With pressure measurement, over-voltage protection and under-voltage compensation system; Automatic compression compensation program control ensures that the flow accuracy of the pump is stable when it works at high pressure.

The precision of the pump is high, so a special filter is added at the inlet end of the pump to prevent the fine hard particles from damaging the plunger and affecting the normal use. Its main technical indicators are as follows:

Flow range: 0.01-9.99ml/min.

Working pressure: 0 ~ 40 MPa

Repetition accuracy%: 1

Flow accuracy%: 3

Pipeline valve:

The pipeline valve and taper seal in the connection section between the pump and the container are made of φ8 series parts with pressure resistance of 50MPa and 316L, so as to ensure the corrosion resistance of the process pipeline in this section at room temperature.

4-2, heat exchange system:

The heat exchange system comprise a medium preheater, a constant temperature box and correspond pipeline valve parts.

Medium preheater:

The medium preheater adopts coil water bath circulating heat exchange mode, and the medium coil is coiled by φ8×2mm pipeline, with a pipeline of 10m, a heat exchange area of 0.25M2 and a material of 316.

Water bath heater bath 8L, heating power 1.2kW, hot circulating pump 120W, made of 304 stainless steel, heating temperature room temperature ~ 100℃, the temperature is adjusted and controlled by the control panel instrument. The water bath tank is equipped with a movable liquid level controller. When the liquid level of the water bath tank is lower than the protective liquid level, it will trigger protection, stop heating, and prevent heating components from being damaged. Please check the water level of the water bath tank in advance before using the equipment.

Thermobox:

Front door, built-in spotlights, stainless steel liner, silent axial fan for hot air circulation in the box, A3 phosphating and plastic spraying outside, beautiful and atmospheric. Equipped with casters and supporting feet, it is convenient to move and the positioning level is adjustable.

Adopting PID control technology, the temperature in the box is uniform and the temperature control accuracy is high;

Working temperature: 150℃ 1℃

Size of inner container: 600×450×550㎜ (length× width× height)

Pipeline valve:

The valves and taper seals of this section of pipeline are made of DW8 and pressure-resistant 50MPa series parts, and the materials are selected according to different fluids and temperatures.

The material of the inlet front part of the medium preheater is 316L；; The remaining pipelines adopt 316 pipelines and pipe fittings;

4-3. Back pressure valve:

It is used to control the reaction pressure inside the reactor. It adopts a high-precision pressure control valve with a control pressure of 0-16MPa and a control accuracy of 0.1MPa. The main material is 316L stainless steel.

4-4, temperature control system:

It is mainly used to control the temperature of reaction kettle and incubator, and collect the temperature of main components, which is composed of temperature sensor and temperature digital display secondary instrument.

The temperature sensor is PT100, the measuring range is 0-200℃, and the output signal is 4-20mA.

Digital display secondary instrument: mainly used to display temperature value, which is convenient for later calculation; Domestic high-precision temperature digital display secondary meter is adopted, which has the advantages of high acquisition speed and high accuracy, and has RS485 communication, which can realize communication with computer.

4-5, pressure measurement and display:

Pressure control mainly displays the pressure of the reaction kettle, which consists of two parts: pressure sensor and pressure controller.

The pressure sensor is imported from Switzerland, with a measuring range of 25MPa, an accuracy of 0.1%F.S, a power supply of 9-36V and an output of 4-20mA. The sensor has high accuracy and long-term stability.

The pressure control instrument adopts digital display secondary instrument, which can realize communication with computer; This kind of digital display secondary meter has the advantages of high acquisition speed, high accuracy and so on. With RS485 communication, it can communicate with the computer.

4-6, safety protection system:

All tanks and reaction vessels of the equipment are equipped with pressure gauges and safety valves to protect the pressure and automatically release the pressure.

Water level protection measures are set for water bath heat exchange, and pressure protection measures are set for the main reactor, which triggers safety protection, beeps to remind and automatically cuts off the corresponding power, automatically prevents the increase of internal environment, and returns to normal after manually solving the problem.

4-7, pipe valve system:

Mainly composed of tee joint, cross joint, pipeline, conical seal, etc. Specification: Ф 6-8/50mpa 316, 316L material; The connection structure of pipeline process is compact, the pipeline is beautifully bent and easy to disassemble.

4-8, electrical control system

It mainly includes brand electrical components, controllers and heat sinks, strong and weak cables and shielded cables for control systems. Power wiring adopts three-phase five-wire system, which has high safety.

4-9, box bracket:

It is mainly used to install various components and protective devices in the fixing system. The main frame is made of industrial aluminum profiles, and the high-temperature safety protection and panel display parts are made of stainless steel laser processing.

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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