SFEY-05超临界乙醇干燥设备

一、设备概述
    利用超临界乙醇对凝胶样品进行干燥具有时间短、见效快、操作简单等优点。在选用设备时，超临界二氧化碳干燥工艺是高压低温的过程，而超临界乙醇干燥工艺是高温低压的干燥过程，因两种工艺的条件相差很大，需对凝胶物性进行了解，防止损伤物料。
二、凝胶物料的制备
    将(CH3COO)2Mg·4H2O配制成0.2mol/L水溶液，然后加入3gPEG4000，室温下充分搅拌0.5～1h，缓慢滴加0.4mol/LNaOH溶液至pH9.5，再继续搅拌直至溶胶产生，胶体体系在低温下陈化24h。然后离心分离除去上清液，并用去离子水洗涤3～5次，再用无水乙醇洗涤3～5次，得到醇凝胶。
    将得到的半透明状醇凝胶置于100mL高压釜内,再加入40mL无水乙醇，搅拌均匀以形成乙醇溶胶混合液。用N2吹扫高压釜3次以驱除反应釜中的空气，封釜搅拌并升温,使釜内温度，压力高于乙醇的临界点(温度为243℃，压力为6.7MPa)以上，达到280℃，7.0MPa后维持30min，缓慢释放流体，回到常压，再通入N2吹扫3次以携带出残余的乙醇蒸气，自然冷却至室温，得到干凝胶。将干凝胶放于马弗炉中600℃煅烧3h后自然冷却至室温，得到MgO纳米颗粒。
    乙醇超临界流体干燥技术合成纳米Y2O3颗粒将纯度为99.99%Y2O3粉末溶于分析纯的浓HNO3,加去离子水配制成浓度为0.1mol/LY(NO3)3溶液,称取少量分析纯的(NH4)2SO4和PEG4000添加到Y(NO3)3溶液中,强力搅拌10min后,往溶液缓慢滴加25%氨水,滴定氨水时将反应体系置于低温下进行。当反应体系的pH为9时,停止滴加氨水。继续搅拌溶液4h后,得到前驱物溶胶。将溶胶用去离子水洗涤3次，再用无水乙醇洗涤3次,即获得前驱物凝胶。   
三、乙醇干燥的优越性
    采用乙醇超临界流体干燥（SCFD）技术制备的MgO纳米颗粒对醋酸乙烯蒸气的催化发光强度是普通干燥技术制备的MgO纳米颗粒的6倍；纳米Y2O3对乙酸乙酯蒸气的催化发光强度较Y2O3也提高了约3倍。
    说明应用超临界乙醇干燥技术制备的纳米材料较普通技术制备的纳米材料具有更强的催化活性。利用超临界乙醇干燥技术制备的纳米颗粒设计的检测醋酸乙烯蒸气的催化发光传感器具有灵敏度较高、选择性优异和稳定性好的优点，可满足快速在线检测低浓度醋酸乙烯的要求。
三、主要技术指标：
    工作压力：≤32MPa
    工作温度：室温～300℃
    干燥釜容积：5L/32MPa  DN160×240mm
    分离器容积：2L/30MPa
    电源：AC380V 50Hz   三相五线    8kW

I. Overview of equipment

Using supercritical ethanol to dry gel samples has the advantages of short time, quick effect and simple operation. When selecting equipment, supercritical carbon dioxide drying process is a high-pressure and low-temperature process, while supercritical ethanol drying process is a high-temperature and low-pressure drying process. Because of the great difference between the conditions of the two processes, it is necessary to understand the physical properties of gel to prevent damage to materials.

Second, preparation of gel materials

(CH3COO)2Mg·4H2O was prepared into 0.2mol/L aqueous solution, then 3gPEG4000 was added, and the mixture was fully stirred for 0.5 ~ 1h at room temperature, then 0.4mol/LNaOH solution was slowly dropped to pH9.5, and then stirring was continued until sol was generated, and the colloid system was aged for 24h at low temperature. Then centrifugally separating to remove supernatant, washing with deionized water for 3-5 times, and washing with anhydrous ethanol for 3-5 times to obtain alcohol gel.

The obtained translucent alcohol gel was placed in a 100mL autoclave, and then 40mL anhydrous alcohol was added and stirred evenly to form an ethanol sol mixed solution. Purge the autoclave with N2 for three times to drive out the air in the autoclave, seal the autoclave, stir and raise the temperature, so that the temperature and pressure in the autoclave are higher than the critical point of ethanol (temperature is 243℃, pressure is 6.7MPa), reach 280℃, and keep it at 7.0MPa for 30min, then slowly release the fluid, return to normal pressure, blow in N2 for three times to carry out the residual ethanol vapor, and naturally cool to room temperature to obtain xerogel. The xerogel was calcined in a muffle furnace at 600℃ for 3 hours and then naturally cooled to room temperature to obtain MgO nanoparticles.

Synthesis of nanometer Y2O3 particles by ethanol supercritical fluid drying technology: Y2O3 powder with purity of 99.99% was dissolved in analytically pure concentrated HNO3, and deionized water was added to prepare a solution with concentration of 0.1mol/LY(NO3)3. A small amount of analytically pure (NH4)2SO4 and PEG4000 were weighed and added to the solution of Y(NO3)3, and after being vigorously stirred for 10min, 25% ammonia water was slowly dropped into the solution. When the pH of the reaction system is 9, the dropping of ammonia water is stopped. After stirring the solution for 4 hours, the precursor sol was obtained. Washing the sol with deionized water for three times, and then washing with anhydrous ethanol for three times to obtain the precursor gel.    

Third, the advantages of ethanol drying

The catalytic luminescence intensity of MgO nanoparticles prepared by ethanol supercritical fluid drying (SCFD) technology for vinyl acetate vapor is 6 times that of MgO nanoparticles prepared by ordinary drying technology. The catalytic luminescence intensity of nano Y2O3 for ethyl acetate vapor is also about 3 times higher than that of Y2O3.

It shows that the nano-materials prepared by supercritical ethanol drying technology have stronger catalytic activity than those prepared by ordinary technology. The catalytic luminescence sensor designed by using nanoparticles prepared by supercritical ethanol drying technology to detect vinyl acetate vapor has the advantages of high sensitivity, excellent selectivity and good stability, which can meet the requirements of rapid on-line detection of low concentration vinyl acetate.

Third, the main technical indicators:

Working pressure: ≤32MPa

Working temperature: room temperature ~ 300℃

Drying kettle volume: 5L/32MPa DN160×240mm.

Separator volume: 2L/30MPa

Power supply: AC380V 50Hz tn-s 8kW.

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：
    超临界二氧化碳萃取设备、超临界气凝胶干燥设备、超临界细微粒子制备装置、超临界清洗发泡装置、超临界抗溶剂结晶装置、高温高压磁搅拌反应装置、超临界相平衡仪等。
    岩心自动剖切机、岩心钻取机、岩心钻切机、液氮冷冻钻取机、液氮冷冻切割机、疏松岩心装备装置、岩心端面切磨机、岩心端面切割机、台式切片机、切样机、岩矿切片机、磨片机、单、双盘金相岩相抛光机、颚式破碎机、自动研磨机、岩心快速洗油仪、填砂压实装置、人造岩心制作装置、含粘土人造岩心制作装置、岩心﹙油、水﹚抽空加压饱和实验装置、渗透率自动测定仪、气体渗透率测定仪、全直径岩心渗透率测定仪、克氏渗透率测定仪、氦孔隙度自动测定仪、气体孔隙度测定仪、全直径孔隙度测定仪、气体孔渗联测仪、致密岩心孔渗测定仪、全直径孔渗联测仪、高温覆压孔渗测定仪、岩心饱和度干馏仪、煤岩心测量系统、岩心饱和度干馏仪、全直径岩心饱和度测定仪﹙蒸馏法﹚、碳酸盐含量测定仪﹙表压式﹚、碳酸盐含量测定仪﹙数显式﹚、岩石比面测定仪、岩心流动试验仪、低渗敏感性评价仪、长岩心梯度流动试验仪、特低渗岩心启动压力梯度测量系统、岩心声波综合测试仪、岩心声电渗参数测定仪、岩心电阻率参数测定仪、多功能岩心驱替装置、润湿性测定仪、高压半渗透隔板仪、油、水相对渗透率测定仪、气液相对渗透率仪、高温高压相对渗透率自动测定仪、岩心孔隙铸体仪、岩心力学性能测试系统、长岩心物理模型、多功能综合驱油装置、多维多功能化学驱物理模拟系统、全自动长岩心双管试验装置、聚合物续凝实验装置、天然气水合物的形成及开采、蒸汽驱油试验装置、超临界CO2驱油实验装置、泡沫驱多功能物理模拟实验装置、微观驱物理模拟装置、多层长岩心驱替装置、油藏条件下多功能驱替系统、一维火烧油层实验装置、三维火烧油层实验装置、采油化学剂评价实验装置、天然气水合物抑制评价实验装置、微生物驱油试验装置、振动采油室内模拟试验装置、凝胶转变压力测定仪、全自动过滤因子测定装置、混相仪、动态结垢评价仪、微型蒸汽发生器、油水自动计量装置、油气水自动计量装置、油气水三相自动计量装置、岩心酸化流动试验仪、压裂酸化工作液动滤失仪、堵水调剖流动性能评价仪、支撑剂裂缝导流测试系统、酸蚀裂缝导流仪、酸岩反应旋转岩盘仪、智能高温高压页膨胀仪、高温高压失水仪、动态高温高压养护釜、井壁稳定性模拟实验装置、钻井液高温高压密度特性实验装置、高温高压动态堵漏模拟装置、地层流体高压物性分析仪、深井取样器、原油快速脱水器、原油动态结蜡仪、原油含蜡测定仪、铜板腐蚀试验仪、挂片动态腐蚀仪、活塞式高压配样器、活塞式储样筒、储样筒、岩心夹持器、多测压点岩心夹持器、电阻率岩心夹持器、声电渗岩心夹持器、高温高压岩心夹持器、全直径岩心夹持器、金属填砂模型管、长岩心模型、非金属填砂模型管、径向流岩心夹持器、碳酸盐测定夹持器、孔隙度测定夹持器、动滤失岩心夹持器、双渗模型、达西定律模型、平面径向流模型、一维线性流模型、水电模拟实验装置、ZR中间容器、HC活塞耐酸容器、有机玻璃容器、高压观察窗容器、高温高压反应釜、视窗反应釜、压力调节器、回压阀、手动计量泵、手摇泵、电动计量泵、高压恒速泵、恒压恒速泵、双缸气体增压泵、采样器、加氢高压微反装置、小型固定流化床反应装置、催化反应设备、液固非均相催化反应装置、催化剂反应活性评价装置。
    高压水平阀、垂直阀、三通阀、四通阀、六通阀、单向阀、变丝接头、保护接头、死堵、接管压帽、卡环、仪表接头、高压快速接头、软管接头、取样器转样接头、内卡套过滤器、气瓶接头、手拧式快速接头、双卡套直通球阀、双卡套角式球阀、双卡套快开阀、软密封四通管接头、卡套式直通截止阀、卡套式直通节流止阀、卡套式角式截止阀、卡套式角式节流阀、卡套式角式截止阀、卡套式拧入管接头、卡套式焊接管接头、卡套式中间三通管接头、岩心夹持器专用皮套等。