WO2016004771A1 - 有机固体材料连续蒸馏浇注成型装置 - Google Patents

有机固体材料连续蒸馏浇注成型装置 Download PDF

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WO2016004771A1
WO2016004771A1 PCT/CN2015/074264 CN2015074264W WO2016004771A1 WO 2016004771 A1 WO2016004771 A1 WO 2016004771A1 CN 2015074264 W CN2015074264 W CN 2015074264W WO 2016004771 A1 WO2016004771 A1 WO 2016004771A1
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vessel
distillation
casting
solid material
organic solid
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PCT/CN2015/074264
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English (en)
French (fr)
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李哲
陈金鑫
蔡丽菲
鲁锦鸿
戴雷
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广东阿格蕾雅光电材料有限公司
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/82—Purification; Separation; Stabilisation; Use of additives
    • C07C209/84—Purification
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00—Compounds containing amino groups bound to a carbon skeleton
    • C07C211/43—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton
    • C07C211/57—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings being part of condensed ring systems of the carbon skeleton
    • C07C211/58—Naphthylamines; N-substituted derivatives thereof

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  • the invention relates to a purification and molding device for a chemical material, in particular to a purification casting molding device for an organic solid (photoelectric) material, in particular to a continuous distillation casting molding device for a liquid organic organic material in a vacuum heating state, It has the advantages of lower equipment cost, faster purification, higher yield, less energy consumption, less dust hazard and increased material addition in the vapor deposition crucible.
  • the first category is the transformation process of “solid-gas-solid”
  • the second category is the transformation process of “solid-liquid-gas-solid (liquid)”.
  • the first type of material is not sublimed directly through the liquid state, such as the commonly used electron transport material AlQ 3 .
  • the second type of material is also widely existed.
  • the purification process of the material of the triarylamine in the sublimation instrument belongs to the second type of transformation process, and the gasification temperature Te of the material is higher than the melting point Tm.
  • the vaporized material will condense in the region between the temperature between Te and Tm, and will exist in liquid form, which will easily cause the liquid to flow to other areas and be contaminated.
  • the glass transition temperature of such materials is usually greater than room temperature, so the liquid will agglomerate after condensation, which causes difficulties in product collection, grinding and dispensing.
  • the conventional distillation purification method is directed to substances that are liquid at normal temperature and pressure, such as alcohol, oil, seawater, and the like. Such materials only need to heat the liquid at a lower temperature and under reduced pressure, and the pure components of different components are distilled in order from the lowest to the highest boiling point, and are separately collected by condensation to achieve a purification effect.
  • Industrial distillation equipment for these liquid materials has matured, but such liquid-oriented distillation apparatus and processes are not suitable for the purification of solid organic materials.
  • distillation equipment for solid materials in the industry such as lithium and zinc distillation equipment, and molecular distillation equipment. Preparation, but because these devices are complex in structure, bulky, and costly, they do not have good economics for the purification of organic solid (photoelectric) materials.
  • the current organic photoelectric materials are mostly prepared by vacuum evaporation, and for the vacuum evaporation production line, it is required to increase the amount of the material in the vapor deposition crucible as much as possible to reduce the frequency of adding materials and prolong the production time.
  • the density is small in the powder state.
  • a conventional hole transporting material NPB powder is added to the vapor-deposited crucible to a half full state, and after the heating is started to start vapor deposition, the volume is immediately reduced to about a quarter of the crucible volume.
  • the present invention provides a continuous distillation casting molding apparatus and a corresponding use method, in view of the above-mentioned problem of purification and use of an organic photoelectric material having a gasification temperature (Te) close to or greater than a melting point (Tm) thereof in a vacuum heating state, the present invention provides a continuous distillation casting molding apparatus and a corresponding use method, the apparatus Different from the above cryogenic liquid distillation and high temperature metal distillation unit.
  • the purification device of the present invention the economic efficiency (equipment cost, purification rate, yield, energy consumption) of producing the same amount and purity of the organic photoelectric material is better than that of the sublimation device; and the obtained product form is a high-purity, high-density block.
  • the solidified ingot can increase the material addition quality in the evaporation line of the production line compared with the powder material, and can avoid the dust hazard during the use of the sublimation scraper, the material packaging and the material use.
  • a continuous distillation casting device and a purification method for an organic photoelectric material having a vaporization temperature (Te) close to or greater than a melting point (Tm) and a boiling point (Tb) less than a decomposition temperature (Td) in a vacuum heating state are as follows The technical solution realized:
  • An organic solid material continuous distillation casting molding apparatus comprising a solid liquefaction vessel, a distillation vessel, a product collection vessel, an impurity collection vessel, a vacuum system, and a heating temperature control system, the vacuum system passing through the pipeline and the distillation vessel, the product collection vessel, and the impurity collection
  • the container is in communication
  • the heating temperature control system controls a temperature in the solid liquefaction vessel, the distillation vessel, the product collection vessel, the product collection vessel has a casting mold
  • the solid liquefaction vessel passes through the high temperature valve and the distillation vessel in the pipeline
  • the organic solid material is any organic solid material that must first be converted into a liquid state when sublimated under vacuum.
  • the high temperature valve is a ball valve, a shutoff valve or a flapper valve.
  • the vacuum system includes a mechanical pump, a diffusion pump, and a molecular pump.
  • the distillation vessel, the product collection vessel, and the impurity collection vessel are sequentially connected through a pipeline.
  • the vacuum system is connected to the impurity collecting container through a pipe.
  • the line between the distillation vessel and the product collection vessel is a short distillation head.
  • the solid liquefaction vessel is in communication with a shielding gas storage tank.
  • the heating temperature control system also controls the temperature of the impurity collection container.
  • the heating device of the heating temperature control system is a heating belt, a heating rope, a heating furnace, a heating sleeve, an infrared radiation heating, a heating agitator or a heating package.
  • the material of the solid liquefaction vessel, the distillation vessel, the product collection vessel, the casting mold, and the impurity collection vessel is glass, quartz, metal, ceramic or graphite.
  • the solid liquefaction vessel is heated, liquefied and insulated under a protective atmosphere (inert gas) to replenish the raw materials in the distillation vessel; the solid liquefaction vessel and the distillation vessel are connected by a special high temperature valve at one end.
  • the liquid material is sucked into the distillation vessel under the pressure difference environment of the shielding gas and the other end is vacuum; the liquid material is heated in the distillation vessel at a step temperature, and the low boiling point (or low sublimation temperature) impurities and the higher boiling point product are sequentially successively Distilling;
  • the product collection vessel is heated and maintained at a temperature above the melting point of the product and the boiling point (or sublimation temperature) of the impurity below the boiling point of the product, allowing the vapor of the product to condense into a liquid for collection in a casting mold
  • the impurities are driven away to the impurity collection container; the impurity collection container is at a sufficiently low temperature (room temperature or lower) which is lower than the boiling point (or
  • the apparatus of the present invention is suitable for the distillation purification of any organic solid material which must first be converted to a liquid state when sublimated under vacuum.
  • the functional units such as the solid liquefaction vessel, the distillation vessel, the product collection vessel, the impurity collection vessel, the casting molding die, the vacuum system, the heating temperature control system, etc. may be different parts that are spatially separated, may be a whole, or may be arbitrarily used in other manners. A combination of forms.
  • the solid liquefaction vessel and the distillation vessel are connected by a pipeline, and the pipeline is controlled by a high temperature valve, and the high temperature valve can be used, but not limited to, a ball valve, a shutoff valve, a flapper valve, and the like.
  • the shielding gas may be nitrogen, argon, or other gas inert to the purification material.
  • the distillation vessel is heated in a stepwise manner, and the impurities of low boiling point (or low sublimation temperature) and the products of higher boiling point are successively distilled (sublimed), and the product vapor is condensed into a liquid in the product collection container and flows into the casting mold.
  • the product collection container is kept above the boiling temperature of the low boiling impurities, and the impurities can only be condensed in the impurity collecting container;
  • the second type of impurities are first distilled (sublimed) at a temperature higher than the boiling point of the product, and allowed to condense in the impurity collecting container. After the second type of impurities have been removed, the temperature of the distillation vessel is raised to the boiling point of the product, and the product is distilled off and condensed in the product collection vessel. The first type of impurities cannot be distilled and remain in the distillation vessel.
  • the continuous solidification casting molding device for organic solid materials of the invention has the advantages of lower equipment cost, faster purification speed, higher yield, less energy consumption and less dust hazard than the sublimation equipment commonly used for purifying solids in the electronics industry. And a high-density ingot product that is more suitable for an evaporation line can be obtained.
  • Figure 1 is a schematic view showing the structure of a continuous distillation casting molding apparatus for an organic solid material according to the present invention
  • Figure 3 is the volume ratio of the NPB ingot of the present invention to the NPB powder at the same quality
  • the NPB ingot is on the left and the NPB powder on the right.
  • 1 Solid liquefaction vessel
  • 2 distillation vessel
  • 3 product collection vessel
  • 4 casting mould
  • 5 impurity collection vessel
  • 6 high temperature valve
  • 7 liquid transport pipe
  • 8 short distillation head
  • 9 impurity Export tube
  • 10 - vacuum system 11 - heating temperature control system.
  • the continuous solid material pouring and molding apparatus using the organic solid material of the present invention comprises a solid liquefaction vessel 1, a distillation vessel 2, a product collection vessel 3, an impurity collection vessel 5, a vacuum system 10, and an external connection which are sequentially connected.
  • the heating temperature control system 11 each independently controls the temperature in the solid liquefaction vessel 1, the distillation vessel 2, and the product collection vessel 3.
  • the solid liquefaction vessel 1 and the distillation vessel 2 are connected by a liquid transport pipe 7, and the liquid transport pipe 7 has a high temperature valve 6.
  • the high temperature valve 6 When the high temperature valve 6 is opened, the two vessels are connected, and under the action of the vacuum system 10, the liquid passes through the liquid.
  • the transport pipe 7 flows from the solid liquefaction vessel 1 into the distillation vessel 2; between the distillation vessel 2 and the product collection vessel 3 is a special short distillation head 8 which ensures that the steam distilled from the distillation vessel 2 is distilled from the short distillation head 8 to the product.
  • a protective gas storage tank (not shown) may be connected to the solid liquefaction vessel 1 to operate the distillation system under protective gas.
  • the distillation process can be continuously performed, and the product is collected in the liquid casting molding die 4, and the purified block ingot product can be directly put into the vapor deposition crucible, and the ingot density is large, and the product weight is contained. More, no frequent feeding, reducing labor intensity, improving work efficiency, and avoiding pollution caused by existing dust feeding.
  • NPB is a solid at room temperature, its melting point is about 280 ° C, and the crude product has a purity of 97.5%, which requires a purity of 99.5% or more by distillation.
  • the specific operation method is as follows.
  • the solid liquefaction vessel 1 is evacuated and flushed with nitrogen gas, and the operation is repeated three times to ensure that the NPB in the solid liquefaction vessel 1 is sufficiently protected from being oxidized upon heating.
  • the heating temperature control system 11 is turned on, the temperature of the solid liquefaction vessel 1 is set at 350 ° C, the temperature of the distillation vessel 2 is set at 350 ° C, and the temperature of the product collection vessel 3 is set at 320 ° C (it should be noted that the actual temperature of the liquid to be heated) The temperature will be somewhat less than the set temperature.)
  • the temperature of the distillation vessel 2 is gradually raised to 450 ° C to boil the NPB liquid in the distillation vessel 2, and the short distillation head 8 is sufficiently heated and kept warm so that the NPB vapor can enter the product collection vessel 3.
  • the whole distillation process lasted for about 4 hours.
  • the cost of the whole distillation system was 55,000 RMB, and the power consumption was 6 degrees.
  • the bulk NPB pure product was obtained 250g, and the purity by HPLC was 99.7%.
  • Comparative Example In order to verify the advantages of the continuous solids casting molding apparatus for organic solid materials of the present invention, the same batch of 300 g NPB was sublimed and purified using a sublimation instrument of a certain type (cost of about 500,000 RMB). The sublimation of 300g NPB took 24 hours and consumed about 40 degrees. Finally, 240g of powder with the same purity of 99.7% was obtained.
  • the pure product obtained by the continuous distillation casting molding device of organic solid material is a block ingot, which is very convenient to obtain and transfer; and the pure NPB obtained by sublimation is powder, and a large amount of dust is collected during the scraping and transferring process of the product. Floating or adhering is not conducive to product handling and personnel health.
  • the bulk NPB ingot obtained by continuous distillation casting of organic solid material was compared with the same quality NPB powder: the same mass of NPB ingot and NPB powder were added to two containers of the same diameter, and then compared.
  • the volume (height) occupied by the NPB powder is found to be 2.5 to 3 times the volume of the same quality NPB ingot (see Figure 3). This comparison shows that for the same volume of bismuth, the use of NPB ingots can be higher.
  • the amount of material added is more conducive to prolonging the production time of the evaporation line and improving economic efficiency.
  • the continuous distillation casting molding device of the organic solid material of the invention has lower equipment cost, faster purification speed, higher yield, less energy consumption and dust hazard than the sublimation equipment commonly used for purifying solids in the electronics industry. Smaller advantages and a high-density ingot product that is more suitable for the evaporation line.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

本发明涉及有机固体材料连续蒸馏浇注成型装置，包括固体液化容器、蒸馏容器、产物收集容器、杂质收集容器、真空系统和加热控温系统，所述真空系统通过管路与蒸馏容器、产物收集容器、杂质收集容器连通，所述加热控温系统控制固体液化容器、蒸馏容器，产物收集容器中的温度，所述产物收集容器中有浇注成型模具，所述固体液化容器通过管路中的高温阀门与蒸馏容器连通，所述有机固体材料为任何于真空状态下升华时必先转变为液态的有机固体材料。本发明装置相对于电子工业中纯化固体常用的升华设备，具有设备成本更低、纯化速度更快、产率更高、耗能更少、粉尘危害更小的优势，并且可以获得更加适合于蒸镀生产线的高密度铸锭产品。

Description

有机固体材料连续蒸馏浇注成型装置 技术领域
本发明涉及一种化学材料的纯化成型装置，特别是涉及一种有机固体(光电)材料的纯化浇注成型装置，尤其是针对在真空加热状态下存在液态的有机光电材料的连续蒸馏浇注成型装置，具有设备成本更低、纯化速度更快、产率更高、耗能更少、粉尘危害更小以及可增加蒸镀坩埚内材料添加量的优势。
背景技术
近年来随着有机光电材料的发展，对固体类有机材料的大规模纯化设备和方法又提出来了更高的要求。常用的固体有机材料纯化方法有重结晶、过层析柱、溶剂洗涤等，但这些方法已经不适用于有机光电类材料的提纯要求，因为通过这些化学纯化方法获得的材料难以达到99.5％以上的高纯度，而且材料中残留的溶剂会对有机光电器件的真空制程产生不良影响。所以国内外材料生产商普遍采用升华的方法来纯化材料以达到有机电子工业对材料高纯度的要求。
然而，由于物质物理性质的不同，固体有机材料在利用升华仪纯化过程中经历的物理过程也存在区别，大致上可以分为两类：第一类为“固体—气体—固体”的转变历程；第二类为“固体—液体—气体—固体(液体)”的转变历程。第一类物质不经过液态直接升华，例如常用的电子传输材料AlQ3。而第二类物质也广泛存在，例如三芳基胺类的材料在升华仪中的纯化过程属于第二类转变历程，该类材料的气化温度Te要高于熔点Tm。这类物质通过升华仪提纯往往存在一些问题：一方面气化的材料在温度介于Te和Tm之间的区域冷凝下来之后，会以液体形式存在，容易造成液体串流到其它区域而被污染；另一方面该类材料的玻璃化转变温度通常要大于室温，因此液体冷凝后会结块，造成产品收集、研磨和分装方面的困难。
由于这类Tm<Te类型的固体在加热后会转变成液态，因此考虑采用蒸馏的方式来纯化此类物质。但是，传统的蒸馏纯化方法针对的是常温常压下为液体的物质，例如酒精、油类、海水等。这类物质只需在较低温度、减压条件下对液体进行加热，不同成分的纯品即会按照沸点由低到高的顺序依次被蒸馏出，通过冷凝进行分别收集，达到纯化效果。针对这些液体类物质的工业蒸馏设备已经十分成熟，但这类针对液体的蒸馏装置和工艺不适合固体类有机物的纯化。工业上也有针对固体物质的蒸馏设备，例如锂、锌的蒸馏设备，以及分子蒸馏设 备等，但因为这些设备结构复杂、体积庞大、成本高昂,对于有机固体(光电)材料的纯化不具有好的经济性。
另外，目前的有机光电材料多以真空蒸镀的方式制备成器件，对于真空蒸镀生产线，要求尽可能增加蒸镀坩埚内材料的添加量，以减少添加材料的频率和延长生产时间。对于真空加热状态下存在液态的材料，其在粉末状态下密度都较小。例如，将一种常用的空穴传输材料NPB粉末添加于蒸镀坩埚内至半满状态，开启加热开始蒸镀之后，其体积立即缩减为坩埚体积的四分之一左右。
发明内容
针对上述在真空加热状态下的气化温度(Te)接近或大于其熔点(Tm)的有机光电材料的提纯和使用问题，本发明专利提供一种连续蒸馏浇注成型装置和相应使用方法，该装置有别于上述的低温液体蒸馏和高温金属蒸馏装置。采用本发明的纯化装置，生产同样数量和纯度的有机光电材料的经济效益(设备成本、纯化速度、产率、能源消耗)要好于升华装置；且获得的产品形式是高纯度、高密度的块状凝固铸锭，相比粉末材料可增加生产线蒸镀坩埚内的材料添加质量，可避免升华刮管、材料分装、材料使用过程中的粉尘危害。
一种针对在真空加热状态下的气化温度(Te)接近或大于其熔点(Tm)、沸点(Tb)小于分解温度(Td)的有机光电材料的连续蒸馏浇注成型装置和纯化方法是通过以下技术方案实现的：
有机固体材料连续蒸馏浇注成型装置，包括固体液化容器、蒸馏容器、产物收集容器、杂质收集容器、真空系统和加热控温系统，所述真空系统通过管路与蒸馏容器、产物收集容器、杂质收集容器连通，所述加热控温系统控制固体液化容器、蒸馏容器，产物收集容器中的温度，所述产物收集容器中有浇注成型模具，所述固体液化容器通过管路中的高温阀门与蒸馏容器连通，所述有机固体材料为任何于真空状态下升华时必先转变为液态的有机固体材料。
所述高温阀门为球阀、截止阀或挡板阀。
所述真空系统包括机械泵、扩散泵、分子泵。
所述蒸馏容器、产物收集容器、杂质收集容器通过管路依次相连通。
所述真空系统通过管路连接于杂质收集容器上。
所述蒸馏容器与产物收集容器之间的管路为短蒸馏头。
所述固体液化容器与保护气体贮气罐相连通。
所述加热控温系统还控制杂质收集容器的温度。
所述加热控温系统的加热装置为加热带、加热绳、加热炉、加热套、红外线辐射加热、加热搅拌器或加热包。
所述固体液化容器、蒸馏容器、产物收集容器、浇注成型模具、杂质收集容器的材质为玻璃、石英、金属、陶瓷或石墨。
固体液化容器对待纯化的固体在保护气氛下(惰性气体)进行加热液化和保温，可对蒸馏容器内的原料进行补充；固体液化容器和蒸馏容器之间采用特殊的高温阀门进行连接，在一端为保护气体、另一端为真空的压差环境下，液态原料被吸入蒸馏容器；液体原料在蒸馏容器内按阶梯温度被加热，依次将低沸点(或低升华温度)的杂质和较高沸点的产品蒸出；产物收集容器被加热并保持在一定温度，该温度高于产物的熔点和杂质的沸点(或升华温度)而低于产物的沸点，使产物的蒸汽冷凝为液体收集在浇注成型模具中，杂质则被驱离至杂质收集容器；杂质收集容器处于足够低的温度(室温或更低温度)，该温度低于杂质的沸点(或升华温度)，杂质在此冷凝；固体液化容器，蒸馏容器、产物收集容器和杂质收集容器依次相连通，真空系统连接于杂质收集容器的末端，同样为蒸馏容器和杂质收集容器提供高真空，降低产物和杂质的沸点(或升华温度)，所述真空系统由机械泵、扩散泵、分子泵产生真空；加热控温系统为整个装置提供加热，将各部分维持在合适的独立的温度区间，杂质收集容器可以加热也可以不加热，优选不加热的情况，其加热装置可以采用但不限于加热带(绳)、加热炉、加热套、红外线辐射加热、加热搅拌器、加热包等。
本发明装置适用于任何于真空状态下升华时必先转变为液态的有机固体材料的蒸馏纯化。
固体液化容器、蒸馏容器、产物收集容器、杂质收集容器、浇注成型模具、真空系统、加热控温系统等功能单元可以是空间上分立的不同部分，也可以是一个整体，或者是采用其他方式任意组合而成的形式。
固体液化容器与蒸馏容器之间通过管路连接，管路上通过高温阀门控制其连通，高温阀门可以采用但不限于球阀、截止阀、挡板阀等。
固体液化容器、蒸馏容器、产物收集容器、浇注模具、杂质收集容器的材质可以采用但不限于玻璃、石英、金属、陶瓷、石墨等耐热材料，容器及浇注模具可以采用各类形状。
保护气体可以是氮气、氩气，或其他对提纯物质具有惰性的气体。
有机固体材料连续蒸馏浇注成型装置操作步骤如下：
(1)在固体液化容器内加入待纯化的物料，排除其中的空气后通入保护气体，同时将蒸馏容器、产物收集容器、杂质收集容器抽至高真空(<10Pa)；
(2)开启加热控温系统，将固体液化容器、蒸馏容器、产物收集容器加热至比熔点稍高的温度；
(3)打开高温阀门，液化的物料从固体液化容器被吸入蒸馏容器，待蒸馏容器内的物料达到其容积的1/3至1/2时关闭高温阀；
(4)蒸馏容器按阶梯方式加热升温，先后蒸馏(升华)出低沸点(或低升华温度)的杂质和较高沸点的产物，产物蒸汽在产物收集容器中冷凝成液体并流入浇注成型模具中，产物收集容器保持在低沸点杂质的沸点温度以上，杂质仅能冷凝于杂质收集容器中；
(5)待蒸馏容器内大部分物料蒸馏掉之后，重复以上(3)、(4)步骤，实现连续化蒸馏作业，最后降温获得高纯度块状铸锭。
工作原理：目前有机光电材料大部分是具有一定共轭程度的小分子化合物，工业上合成此类共轭小分子一般采用金属催化反应，产物中的杂质主要是在合成过程中引进或残留。根据仪器分析，杂质主要分为两类：一类是金属催化剂，该类杂质难以升华或者蒸馏，是高温纯化过程的主要残留物；另一类是催化反应进行不彻底而残留下的分子量较小的中间产物，该类杂质比产物的分子量更小，更容易被蒸馏或者升华。针对以上两类杂质，先在较高但低于产物沸点的温度，将第二类杂质蒸馏(升华)出来，让其冷凝在杂质收集容器。第二类杂质除尽之后，升高蒸馏容器温度达到产物沸点，让产物蒸馏出并在产物收集容器冷凝。第一类杂质无法蒸馏而残留在蒸馏容器。
本发明有机固体材料连续蒸馏浇注成型装置，相对于电子工业中纯化固体常用的升华设备，具有设备成本更低、纯化速度更快、产率更高、耗能更少、粉尘危害更小的优势，并且可以获得更加适合于蒸镀生产线的高密度铸锭产品。
附图说明
图1本发明的有机固体材料连续蒸馏浇注成型装置结构示意图，
图2本发明的有机固体材料连续蒸馏浇注成型装置中加热温控系统，
图3本发明的NPB铸锭与NPB粉末在相同质量情况下占用体积比，
其中左边为NPB铸锭，右边为NPB粉末，
附图中的标号表示含义如下：
1—固体液化容器，2—蒸馏容器，3—产物收集容器，4—浇注成型模具，5—杂质收集容器，6—高温阀门，7—液体输运管，8—短蒸馏头，9—杂质导出管，10—真空系统，11—加热温控系统。
具体实施方式
如图1、图2所示，利用本发明的有机固体材料连续蒸馏浇注成型装置包括依次连接的固体液化容器1、蒸馏容器2、产物收集容器3、杂质收集容器5、真空系统10，以及外接的加热控温系统11，所述加热控温系统11各自独立控制固体液化容器1、蒸馏容器2，产物收集容器3中的温度。
固体液化容器1、蒸馏容器2之间通过液体运输管7连通，并且液体运输管上7有高温阀门6，当高温阀门6打开时，两容器连通，在真空系统10的作用下，液体经由液体运输管7从固体液化容器1流入到蒸馏容器2中；蒸馏容器2、产物收集容器3之间为特制短蒸馏头8，保证从蒸馏容器2蒸出的蒸汽从短蒸馏头8蒸出到产物收集容器3或杂质收集容器5，产物馏出流入到产物收集容器3中的浇注成型模具4；产物收集容器3、杂质收集容器5之间有杂质导出管9，杂质从蒸馏容器2经短蒸馏头8蒸出后，由于产物收集容器3的温度较高，不会冷凝在产物收集容器3中，而是冷凝在杂质收集容器5内。
固体液化容器1上可以连接保护气体贮气罐(未示意出)，使蒸馏系统在保护气下工作。
通过固体液化容器1的设计，使得蒸馏过程可以连续进行，同时产物收集在液体浇注成型模具4，可以将纯化好的块状铸锭产品直接投入蒸镀坩埚，其铸锭密度大，盛装产物重量多，不用频繁加料，减小了劳动强度，提高了工作效率，同时避免了现有的粉尘投料而造成的污染。
操作实施例：对300g OLED空穴传输材料NPB粗品进行纯化。
NPB在室温下为固体，其熔点为280℃左右，粗品的HPLC纯度为97.5％，需要通过蒸馏使其纯度达到99.5％以上。具体的操作方法如下。
(1)在固体液化容器1和蒸馏容器中2分别加入250g、50g的NPB粗品，高温阀门6此时处于关闭状态。
(2)对固体液化容器1抽真空后冲入氮气，反复进行三次操作，以保证固体液化容器1内的NPB被充分保护，防止加热时被氧化。
(3)打开真空系统10，对蒸馏容器2、产物收集容器3、杂质收集容器5抽真空至50mtorr以下。
(4)打开加热控温系统11，将固体液化容器1温度设置在350℃，蒸馏容器2温度设置在350℃，产物收集容器3温度设置在320℃(应当注意的是，被加热液体的实际温度会一定程度上小于设置温度。)
(5)将蒸馏容器2内液态的粗品NPB在350℃保温10分钟，以除掉低沸点(升华温度)杂质。
(6)将蒸馏容器2温度逐渐升高至450℃，使蒸馏容器2内的NPB液体沸腾，对短蒸馏头8进行充分加热和保温，使NPB蒸汽能够进入产物收集容器3。
(7)持续加热，将蒸馏容器1在450℃进行保温，直到大部分NPB蒸馏完毕。
(8)打开高温阀门6，在一端为保护气体、另一端为真空的压差下，固体液化容器1内的液态NPB粗品被吸入蒸馏容器2内，当固体液化容器1内的NPB减少大概1/5后，关闭高温阀门6。
(9)重复以上第5至第8步的操作，从而进行NPB的连续批次蒸馏。
(10)待NPB蒸馏完毕之后，往各容器内充入氮气使系统自然降温，当温度降至50℃以下后，可以从产物收集容器3内的浇注成型模具4中获得块状铸锭。
整个蒸馏过程持续约4小时，整套蒸馏系统成本为5.5万人民币，耗电6度,获得块状NPB纯品250g，经HPLC检测纯度为99.7％。
对比实施例：为了验证本发明有机固体材料连续蒸馏浇注成型装置的优势，对同一批次的300g NPB利用某型号的升华仪(成本约为50万人民币)进行升华提纯。300g NPB的升华共耗时24小时，耗电约40度,最终获得纯度同样为99.7％的粉末240g。
采用有机固体材料连续蒸馏浇注成型装置获得的纯品为块状铸锭，其获取和转移都极为方便；而采用升华获得的NPB纯品为粉末，产品的刮取、转移过程中有大量的粉尘漂浮或粘附，不利于产品的处理和人员健康。
将有机固体材料连续蒸馏浇注成型装置获得的块状NPB铸锭，与相同质量NPB粉末进行密度对比：往两个相同管径的容器中，分别添加相同质量的NPB铸锭与NPB粉末，然后比较其所占用的体积(高度)，发现NPB粉末占用体积为相同质量NPB铸锭体积的2.5至3倍(见图3)，此对比结果说明，对于相同体积坩埚，使用NPB铸锭可以获得更高的材料添加量，更有利于延长蒸镀生产线的生产时间和提高经济效益。
经过综合比较，本发明有机固体材料连续蒸馏浇注成型装置，相对于电子工业中纯化固体常用的升华设备，具有设备成本更低、纯化速度更快、产率更高、耗能更少、粉尘危害更小的优势，并且可以获得更加适合于蒸镀生产线的高密度铸锭产品。

Claims (10)

  1. 有机固体材料连续蒸馏浇注成型装置，其特征在于：包括固体液化容器、蒸馏容器、产物收集容器、杂质收集容器、真空系统和加热控温系统，所述真空系统通过管路与蒸馏容器、产物收集容器、杂质收集容器连通，所述加热控温系统控制固体液化容器、蒸馏容器，产物收集容器中的温度，所述产物收集容器中有浇注成型模具，所述固体液化容器通过管路中的高温阀门与蒸馏容器连通，所述有机固体材料为任何于真空状态下升华时必先转变为液态的有机固体材料。
  2. 根据权利要求1所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述高温阀门为球阀、截止阀或挡板阀。
  3. 根据权利要求1所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述真空系统包括机械泵、扩散泵、分子泵。
  4. 根据权利要求1所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述蒸馏容器、产物收集容器、杂质收集容器通过管路依次相连通。
  5. 根据权利要求4所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述真空系统通过管路连接于杂质收集容器上。
  6. 根据权利要求4所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述蒸馏容器与产物收集容器之间的管路为短蒸馏头。
  7. 根据权利要求1所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述固体液化容器与保护气体贮气罐相连通。
  8. 根据权利要求1所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述加热控温系统还控制杂质收集容器的温度。
  9. 根据权利要求1所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述加热控温系统的加热装置为加热带、加热绳、加热炉、加热套、红外线辐射加热、加热搅拌器或加热包。
  10. 根据权利要求1所述的有机固体材料连续蒸馏浇注成型装置，其特征在于：所述固体液化容器、蒸馏容器、产物收集容器、浇注成型模具、杂质收集容器的材质为玻璃、石英、金属、陶瓷或石墨。
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1714061A (zh) * 2001-12-15 2005-12-28 Skc株式会社 用于提纯有机电致发光材料的装置和方法
CN102924207A (zh) * 2011-08-13 2013-02-13 广东阿格蕾雅光电材料有限公司 有机小分子升华纯化方法
CN203954714U (zh) * 2014-07-15 2014-11-26 广东阿格蕾雅光电材料有限公司 有机固体材料连续蒸馏装置

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8377264B2 (en) * 2006-12-28 2013-02-19 N.M.G. Environmental Development Co., Ltd Method for disposal of organic waste material and apparatus for the method
CN100584972C (zh) * 2007-11-09 2010-01-27 江西赣锋锂业股份有限公司 金属锂真空蒸馏提纯方法
JP2013116879A (ja) * 2011-10-31 2013-06-13 Idemitsu Kosan Co Ltd 有機材料の精製装置及び有機材料の精製方法
CN204525900U (zh) * 2014-07-11 2015-08-05 广东阿格蕾雅光电材料有限公司 有机固体材料连续蒸馏浇注成型装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1714061A (zh) * 2001-12-15 2005-12-28 Skc株式会社 用于提纯有机电致发光材料的装置和方法
CN102924207A (zh) * 2011-08-13 2013-02-13 广东阿格蕾雅光电材料有限公司 有机小分子升华纯化方法
CN203954714U (zh) * 2014-07-15 2014-11-26 广东阿格蕾雅光电材料有限公司 有机固体材料连续蒸馏装置

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