CN203954714U - Organic solid material continuous distillation plant - Google Patents
Organic solid material continuous distillation plant Download PDFInfo
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- CN203954714U CN203954714U CN201420391435.9U CN201420391435U CN203954714U CN 203954714 U CN203954714 U CN 203954714U CN 201420391435 U CN201420391435 U CN 201420391435U CN 203954714 U CN203954714 U CN 203954714U
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Abstract
The utility model relates to organic solid material continuous distillation plant, it is characterized in that: comprise solid liquefaction vessel, distil container, collection of products container, impurity collection container, vacuum system and heated for controlling temperature system, described vacuum system is by pipeline and distil container, collection of products container, impurity collection container is communicated with, described heated for controlling temperature system control solid liquefaction vessel, distil container, temperature in collection of products container, described solid liquefaction vessel is communicated with distil container by the high temperature valve in pipeline, described organic solid material is anyly must first change liquid organic solid material into while distilling under vacuum state.Distilling apparatus of the present utility model, with respect to the conventional sublimation apparatus of purifying solid in electronics industry, have that equipment cost is lower, purifying speed is faster, productive rate is higher, power consumption still less, advantage that dust harzard is less.
Description
Technical field
The utility model relates to a kind of Novel pure gasifying device of organic solid material, particularly for the extensive continuous batch of distilling apparatus of organic solid material that has liquid phase under heating in vacuum state, utilize this device can make product purity reach more than 99.5% level, and have that equipment cost is lower, purifying speed is faster, productive rate is higher, power consumption still less, dust harzard is less and can increase the advantage of Material Addition amount in evaporation crucible.
Background technology
Along with the development of organic photoelectrical material, large scale purification equipment and method to solid kind organic material have put forward again higher requirement in recent years.Conventional solid organic material purification process has recrystallization, crosses chromatographic column, solvent wash etc., but these methods have not been suitable for the purification requirement of organic photoelectric class material, because the material obtaining by these chemical purification methods is difficult to reach more than 99.5% high-purity, and in material, residual solvent can produce harmful effect to the vacuum process of organic electro-optic device.So manufacture of materials business generally adopts the method for distillation to carry out purified material to reach organic electronic industry to the highly purified requirement of material both at home and abroad.
But due to the difference of physical property of the Earth's materials, solid organic material, utilizing the physical process experiencing in apophorometer purge process also distinct, can be divided into two classes: the transformation course that the first kind is " solid-gas-solid " haply; Equations of The Second Kind is the transformation course of " solid-liquid-gas-solid (liquid) ".First kind material directly distils without liquid state, for example conventional electron transport material AlQ
3.And Equations of The Second Kind material also extensively exists, for example purge process of the material of triaryl amine in apophorometer belongs to Equations of The Second Kind and changes course, and the gasification temperature Te of such material will be higher than fusing point Tm.This class material is purified and is often had some problems by apophorometer: on the one hand the material of gasification in temperature under the region condensation between Te and Tm after, can exist with liquid form, easily cause liquid crossfire to other region and contaminated; The glass transition temperature of such material is greater than room temperature conventionally on the other hand, therefore after condenses, can lump, and causes the difficulty of product-collecting, grinding and packing aspect.
Because the solid of this class Tm<Te type can be transformed into liquid state after heating, therefore consider to adopt the mode of distillation to carry out this type of material of purifying.But, traditional distillation purifying method for be under normal temperature and pressure, to be the material of liquid, such as alcohol, oils, seawater etc.This class material only need heat liquid under lower temperature, reduced pressure, and the sterling of heterogeneity can be distilled out successively according to boiling point order from low to high, collects respectively by condensation, reaches purification effect.Industrial distillation equipment for these liquid substances is very ripe, but this class is not suitable for the organic purifying of solid kind for distilling apparatus and the technique of liquid.The industrial distillation equipment also having for solid matter, the for example distillation equipment of lithium, zinc, and molecular distillation equipment etc., but since these device structure complexity, bulky, with high costs, the economy not had for the purifying of organic solid (photoelectricity) material.
Summary of the invention
Approach or be greater than the purification problem of the organic photoelectrical material of its fusing point (Tm) for above-mentioned gasification temperature (Te) under heating in vacuum state, the utility model patent provides a kind of organic solid material continuous distillation plant, this device is different from above-mentioned cryogenic liquid distillation, high-temperature metal distillation or molecular distillation apparatus, adopt purification devices of the present utility model, the economic benefit (equipment cost, purifying speed, productive rate, energy resource consumption) of producing the organic photoelectrical material of equal number and purity will significantly be better than the method for distillation.
A kind ofly approach or be greater than the organic photoelectrical material that its fusing point (Tm), boiling point (Tb) are less than decomposition temperature (Td) for the gasification temperature under heating in vacuum state (Te), its extensive continuous batch of device that distillation adopts, its technical scheme is as follows:
Organic solid material continuous distillation plant, it is characterized in that: comprise solid liquefaction vessel, distil container, collection of products container, impurity collection container, vacuum system and heated for controlling temperature system, described vacuum system is by pipeline and distil container, collection of products container, impurity collection container is communicated with, described heated for controlling temperature system control solid liquefaction vessel, distil container, temperature in collection of products container, described solid liquefaction vessel is communicated with distil container by the high temperature valve in pipeline, described organic solid material is anyly must first change liquid organic solid material into while distilling under vacuum state.
Described high temperature valve is ball valve, stop valve or flapper valve.
Described vacuum system comprises mechanical pump, diffusion pump, molecular pump.
Described distil container, collection of products container, impurity collection container are connected successively by pipeline.
Described vacuum system is connected on impurity collection container by pipeline.
Pipeline between described distil container and collection of products container is short still head.
Described solid liquefaction vessel is connected with protective gas gas tank.
Described heated for controlling temperature system is also controlled the temperature of impurity collection container.
The heater of described heated for controlling temperature system is heating tape, heating rope, heating furnace, heating jacket, infrared radiation heating, heating stirrer or heat packs.
The material of described solid liquefaction vessel, distil container, collection of products container, impurity collection container is glass, quartz, metal, pottery or graphite.
The utility model solid liquefaction vessel heats liquefaction and insulation to solid to be purified (inert gas) under protective atmosphere, can supplement the raw material in distil container; Between solid liquefaction vessel and distil container, adopt special high temperature valve to connect, at one end, under protective gas, the other end pressure difference environment that is vacuum, liquid material is inhaled into distil container; It is heated that liquid charging stock is pressed step temperature in distil container, successively the impurity of low boiling (or low sublimation temperature) and the product of higher steamed; Collection of products container is heated and remains on uniform temperature, this temperature is higher than the fusing point of product and the boiling point of impurity (or sublimation temperature) and lower than the boiling point of product, the steam-condensation that makes product be liquid collection in casting mold, impurity is expelled to impurity collection container; Impurity collection container is in enough low temperature (room temperature or lower temperature), and this temperature is lower than the boiling point (or sublimation temperature) of impurity, and impurity is in this condensation; Solid liquefaction vessel, distil container, collection of products container and impurity collection container are connected successively, vacuum system is connected in the end of impurity collection container, be similarly distil container and impurity collection container provides high vacuum, reduce the boiling point (or sublimation temperature) of product and impurity, described vacuum system produces vacuum by mechanical pump, diffusion pump, molecular pump; Heated for controlling temperature system provides heating for whole device, each several part is maintained to suitable independently temperature range, impurity collection container can heat also and can not heat, situation about preferably not heating, its heater can adopt but be not limited to heating tape (rope), heating furnace, heating jacket, infrared radiation heating, heating stirrer, heat packs etc.
The utility model device is applicable to any distillation purifying that must first change liquid organic solid material under vacuum state while distilling into.
The functional units such as solid liquefaction vessel, distil container, collection of products container, impurity collection container, vacuum system, heated for controlling temperature system can be different pieces discrete on space, also can be an entirety, or adopt other modes to be combined the form forming.
Between solid liquefaction vessel and distil container, be connected by pipeline, on pipeline, by high temperature valve control, it is communicated with, and high temperature valve can adopt but be not limited to ball valve, stop valve, flapper valve etc.
The material of solid liquefaction vessel, distil container, collection of products container, impurity collection container can adopt but be not limited to the heat proof materials such as glass, quartz, metal, pottery, graphite, and container and casting mold can adopt all kinds of shapes.
Protective gas can be nitrogen, argon gas, or other have the gas of inertia to purifying substances.
Organic solid material continuous still cast-molding device operating procedure is as follows:
(1) in solid liquefaction vessel, add material to be purified, after eliminating air wherein, pass into protective gas, distil container, collection of products container, impurity collection container are evacuated to high vacuum (<10Pa) simultaneously;
(2) open heated for controlling temperature system, solid liquefaction vessel, distil container, collection of products container are heated to the temperature slightly higher than fusing point;
(3) open high temperature valve, the material of liquefaction is inhaled into distil container from solid liquefaction vessel, and the material in container to be distilled reaches the high-temperature valve of closing of its volume at 1/3 to 1/2 o'clock;
(4) distil container is by step-wise manner heat temperature raising, successively distillation (distillation) goes out the impurity of low boiling (or low sublimation temperature) and the product of higher, product vapor is condensed into liquid in collection of products container, more than collection of products container remains on the boiling temperature of low boiling impurity, impurity only can condensation in impurity collection container;
(5) after most of material distills in container to be distilled, repeat above (3), (4) step, realize serialization distillation operation, finally cooling obtains high-purity block product.
Operation principle: organic photoelectrical material major part is the micromolecular compound with certain conjugated degree at present, the industrial synthetic little molecule of this type of conjugation generally adopts metal catalysed reaction, and the impurity in product is mainly introduction or residual in building-up process.According to Instrumental Analysis, impurity is mainly divided into two classes: a class is metallic catalyst, and such impurity is difficult to distillation or distillation, is the main residue of high temperature purification process; Another kind of is the intermediate product that catalytic reaction is carried out the molecular weight under not thorough and residual, and such impurity is less than the molecular weight of product, is more easily distilled or distils.For above two class impurity, first higher but lower than the temperature of product boiling point, by Equations of The Second Kind impurity distillation (distillation) out, allow it be condensate in impurity collection container.After Equations of The Second Kind impurity eliminates, rising distil container temperature reaches product boiling point, allows product distill out and in the condensation of collection of products container.First kind impurity cannot distill and remain in distil container.
The utility model organic solid material continuous distillation plant, with respect to the conventional sublimation apparatus of purifying solid in electronics industry, have that equipment cost is lower, purifying speed is faster, productive rate is higher, power consumption still less, advantage that dust harzard is less, and can obtain the high density ingot casting product that is more suitable for evaporation production line.
Brief description of the drawings
Fig. 1 the utility model organic solid material continuous distillation plant structural representation,
Fig. 2 the utility model organic solid material continuous distillation plant heating control system schematic diagram,
Label in accompanying drawing represents that implication is as follows:
1-solid liquefaction vessel, 2-distil container, 3-collection of products container, 4-impurity collection container, 5-high temperature valve, 6-liquid transport pipe, 7-short still head, 8-impurity delivery line, 9-vacuum system, 10-heating temperature-control system.
Detailed description of the invention
As shown in Figure 1 and Figure 2, utilize organic solid material continuous still cast-molding device of the present utility model to comprise the solid liquefaction vessel 1, distil container 2, collection of products container 3, impurity collection container 4, the vacuum system 9 that connect successively, and external heated for controlling temperature system 10, described heated for controlling temperature system 10 is independent solid liquefaction vessel 1, distil container 2, the temperature in collection of products container 3 controlled separately.
Between solid liquefaction vessel 1, distil container 2, be communicated with by liquid transporting pipe 6, and 6 have high temperature valve 5 on liquid transporting pipe, in the time that high temperature valve 5 is opened, two containers are communicated with, under the effect of vacuum system 9, liquid flow into distil container 2 from solid liquefaction vessel 1 via liquid transporting pipe 6; Between distil container 2, collection of products container 3, be special short still head 7, ensure that the steam steaming from distil container 2 steams collection of products container 3 or impurity collection container 4 from short still head 7, product distillates and flow in collection of products container 3; Between collection of products container 3, impurity collection container 4, there is impurity delivery line 8, impurity from distil container 2 after short still head 7 steams, because the temperature of collection of products container 3 is higher, can not be condensate in collection of products container 3, but be condensate in impurity collection container 4.
In solid liquefaction vessel 1, can connect protective gas gas tank (not illustrating), Distallation systm is worked under protection gas.
By the design of solid liquefaction vessel 1, still-process can be carried out continuously, collection of products exists with bulk form in collection of products container 3 simultaneously, bulk product good purifying directly can be dropped into evaporation crucible, its block density is large, and splendid attire product weight is many, need not frequently feed in raw material, reduce labour intensity, improved operating efficiency, avoided existing dust to feed intake and the pollution that causes simultaneously.
Operation experiments example
As shown in Figure 1, utilize continuous batch of distilling apparatus of the present utility model to carry out purifying to 300g OLED hole mobile material NPB crude product.NPB is at room temperature solid, and its fusing point is 280 DEG C of left and right, and the HPLC purity of crude product is 97.5%, need to its purity be reached more than 99.5% by distillation.Concrete method of operating is as follows.
(1) the 2 NPB crude products that add respectively 250g, 50g in solid liquefier 1 and distiller, high temperature valve 5 is now in closed condition.
(2) pour nitrogen after solid liquefier 1 is vacuumized, repeatedly carry out three operations, to ensure that the NPB in solid liquefier 1 is adequately protected, oxidized while preventing from heating.
(3) open vacuum system 9 intermediate pumps, distiller 2, product collector 3, impurity collector 4 are evacuated to below 50mtorr.
(4) open heated for controlling temperature system 10, solid liquefier 1 temperature is arranged on to 320 DEG C, distiller 2 temperature are arranged on 350 DEG C, and product collector 3 temperature are arranged on 320 DEG C, and (actual temperature that it should be noted in the discussion above that heated liquid can be less than set temperature to a certain extent.)
(5) the crude product NPB of distiller 2 interior liquid state is incubated to 10 minutes at 350 DEG C, to remove low boiling (or low sublimation temperature) impurity.
(6) distiller 2 temperature are increased to 450 DEG C gradually, make the NPB liquid boiling in distiller 2, short still head 7 is fully heated and is incubated, make NPB steam can enter product collector 3.
(7) continuous heating, is incubated distiller 2 at 450 DEG C, until most of NPB distillation is complete.
(8) open high temperature valve 5, at one end, under protective gas, the other end pressure reduction that is vacuum, the liquid NPB crude product in solid liquefier 1 is inhaled in distiller 2, after the NPB in solid liquefier 1 reduces general 1/5, closes high temperature valve 5.
(9) repeat above the 5th operation to the 8th step, thereby carry out the continuity distillation of NPB.
Whole still-process continues approximately 4 hours, and a whole set of Distallation systm cost is about 50,000 RMB, and power consumption approximately 6 degree, obtain NPB sterling 250g, and detecting purity through HPLC is 99.7%.
Comparative example: in order to verify the advantage of the utility model distilling apparatus and purification process, the 300g NPB of same batch is utilized to the purification that distils of the apophorometer (cost is about 500,000 RMB) of certain model.The distillation of 300g NPB 24 hours consuming time altogether, power consumption approximately 40 degree, finally obtain purity and are similarly 99.7% sterling 240g.
The NPB sterling that contrast obtains with different purification process and device, the sterling that adopts distilling apparatus to obtain is block, it obtains and shifts all very convenient; And the NPB sterling that adopts distillation to obtain is powder, in the scraping of product, transfer process, there is a large amount of dust floating or adhere to, be unfavorable for processing and the personnel health of product.
Through comprehensive relatively, distilling apparatus of the present utility model, with respect to the conventional sublimation apparatus of purifying solid in electronics industry, have that equipment cost is lower, purifying speed is faster, productive rate is higher, power consumption still less, advantage that dust harzard is less.
Claims (10)
1. organic solid material continuous distillation plant, it is characterized in that: comprise solid liquefaction vessel, distil container, collection of products container, impurity collection container, vacuum system and heated for controlling temperature system, described vacuum system is by pipeline and distil container, collection of products container, impurity collection container is communicated with, described heated for controlling temperature system control solid liquefaction vessel, distil container, temperature in collection of products container, described solid liquefaction vessel is communicated with distil container by the high temperature valve in pipeline, described organic solid material is anyly must first change liquid organic solid material into while distilling under vacuum state.
2. organic solid material continuous distillation plant according to claim 1, is characterized in that: described high temperature valve is ball valve, stop valve or flapper valve.
3. organic solid material continuous distillation plant according to claim 1, is characterized in that: described vacuum system comprises mechanical pump, diffusion pump, molecular pump.
4. organic solid material continuous distillation plant according to claim 1, is characterized in that: described distil container, collection of products container, impurity collection container are connected successively by pipeline.
5. organic solid material continuous distillation plant according to claim 4, is characterized in that: described vacuum system is connected on impurity collection container by pipeline.
6. organic solid material continuous distillation plant according to claim 5, is characterized in that: the pipeline between described distil container and collection of products container is short still head.
7. organic solid material continuous distillation plant according to claim 1, is characterized in that: described solid liquefaction vessel is connected with protective gas gas tank.
8. organic solid material continuous distillation plant according to claim 1, is characterized in that: described heated for controlling temperature system is also controlled the temperature of impurity collection container.
9. organic solid material continuous distillation plant according to claim 1, is characterized in that: the heater of described heated for controlling temperature system is heating tape, heating rope, heating furnace, heating jacket, infrared radiation heating, heating stirrer or heat packs.
10. organic solid material continuous distillation plant according to claim 1, is characterized in that: the material of described solid liquefaction vessel, distil container, collection of products container, impurity collection container is glass, quartz, metal, pottery or graphite.
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| CN201420391435.9U CN203954714U (en) | 2014-07-15 | 2014-07-15 | Organic solid material continuous distillation plant |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016004771A1 (en) * | 2014-07-11 | 2016-01-14 | 广东阿格蕾雅光电材料有限公司 | Continuous distillation casting device for organic solid material |
| WO2016008313A1 (en) * | 2014-07-15 | 2016-01-21 | 广东阿格蕾雅光电材料有限公司 | Continuous distillation device of organic solid material |
-
2014
- 2014-07-15 CN CN201420391435.9U patent/CN203954714U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016004771A1 (en) * | 2014-07-11 | 2016-01-14 | 广东阿格蕾雅光电材料有限公司 | Continuous distillation casting device for organic solid material |
| WO2016008313A1 (en) * | 2014-07-15 | 2016-01-21 | 广东阿格蕾雅光电材料有限公司 | Continuous distillation device of organic solid material |
| CN105311852A (en) * | 2014-07-15 | 2016-02-10 | 广东阿格蕾雅光电材料有限公司 | Organic solid material continuous distillation device |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: Organic solid material continuous distillation device Effective date of registration: 20181105 Granted publication date: 20141126 Pledgee: Guangdong Nanhai Rural Commercial Bank branch branch of Limited by Share Ltd Pledgor: GUANGDONG AGLAIA OPTOELECTRONIC MATERIALS Co.,Ltd. Registration number: 2018440000305 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |