CN104667562B - Organic material bi-directional vacuum sublimation purification equipment and continuous or non-continuous purifying method - Google Patents
Organic material bi-directional vacuum sublimation purification equipment and continuous or non-continuous purifying method Download PDFInfo
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- CN104667562B CN104667562B CN201510046229.3A CN201510046229A CN104667562B CN 104667562 B CN104667562 B CN 104667562B CN 201510046229 A CN201510046229 A CN 201510046229A CN 104667562 B CN104667562 B CN 104667562B
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Abstract
The invention relates to the technical field of organic material purification equipment and in particular relates to organic material bi-directional vacuum sublimation purification equipment and a continuous or non-continuous purifying method, belonging to the field of the physical vapor deposition technology. The organic material bi-directional vacuum sublimation purification equipment comprises a vacuum cavity, a vacuumizing device and a cooling device, wherein a valve and a quartz tube assembly with openings at two ends are arranged in the vacuum cavity, and the quartz tube assembly can be used for sublimation purification when comprising a collecting section and a heating section, which are connected in series, and can be used for continuous sublimation purification when comprising a coarse sublimation groove, a transitional groove and a deep sublimation groove, which are sequentially connected. The organic material bi-directional vacuum sublimation purification equipment has simple structure, can be operated easily, has high efficiency, and can improve the purity of organic materials while effectively saving the time. The continuous or non-continuous purifying method can remarkably increase the purification purity.
Description
Technical field
The present invention relates to the equipment for purifying technical field of organic material, more particularly, to a kind of organic material bidirectional vacuum distillation
Equipment for purifying and continuously or discontinuously method of purification, belong to technical field of physical vapor deposition.
Background technology
In recent years, the development of mobile interchange and flat pannel display industry, Organic Light Emitting Diode, by its numerous advantage, welcomes
Development as emerging rapidly in large numbersBamboo shoots after a spring rain, of increased attention.Its main advantage have of many uses due to organic material,
Especially on a lot of photoelectric devices, embody good performance, but this be inseparable relation with the purity of organic material,
In organic material, impurity can directly result in electric charge accumulation, forms local current excessive, thus reducing the efficiency of opto-electronic device
And the life-span, the purity of therefore organic material is higher, and performance is also better.But domestic organic material purity relatively low always it is impossible to
Meet the demand of industry at this stage.
Vacuum equipment for purifying for present domestic application is mainly by the way of unidirectional distillation, mainly according to gradient
The process heating up, the process that impurity and target product are gradually disengaged, it is characterised by, the organic compound in sublimation pipe is according to true
The direction diffusion of air stream, the gradient with temperature reduces, and realizes the purification of target substance.But the method is in the mistake heated
Cheng Zhong, in low-temperature region, impurity can be attached on leading portion tube wall during distillation, thus causing impurity and target product
Can not efficiently separate, thus target product can not effectively be purified, meanwhile, the density of organic material is smaller, frequent single
Sample-adding amount can not be effectively accomplished the maximum deposition of apophorometer so that the effectiveness of apophorometer can not be made full use of.If obtained
Obtaining efficiently high-purity target compound needs repeatedly to purify, so we devise a kind of method of two-way sublimation purification, effectively
Solve the method that impurity can not efficiently separate.
Content of the invention
For solving the deficiencies in the prior art, the invention provides a kind of bidirectional vacuum sublimation purification equipment of organic material.
The purpose of the present invention is achieved through the following technical solutions.
A kind of bidirectional vacuum sublimation purification equipment of organic material, including：Vacuum cavity, vacuum extractor and cooling dress
Put, be respectively arranged with the first valve and the second valve at the two ends of described vacuum cavity, in described vacuum cavity, be provided with two
The quartzy tube assembly of end opening；
The described vacuum extractor described chiller of series connection, described chiller described first valve of series connection, described quartz
One opening of tube assembly is near described first valve；
The described vacuum extractor described chiller of series connection, described chiller described second valve of series connection, described quartz
Another opening of tube assembly is near described second valve.
Preferably, described quartz tube assembly includes collection section and the bringing-up section connected, and described collection section is located near described
The side of the first valve, described bringing-up section is located at the side near described second valve.
Preferably, the bidirectional vacuum sublimation purification equipment of described organic material also includes the heating to the heating of described bringing-up section
Device.
Present invention also offers a kind of bidirectional vacuum sublimation purification method of organic material, comprise the steps：
1) organic material is placed in the bringing-up section of quartzy tube assembly, closes the first valve and open the second valve,
It is evacuated to 10-3～10-4After Pa, organic material is heated, temperature control is 20～50 below the sublimation point of organic material
DEG C, constant temperature 40～100 minutes, small-molecular-weight impurity is drawn in chiller.
2) close the second valve, open the first valve, organic material is heated, temperature control is in the liter of organic material
Between above 0～80 DEG C of China's point, constant temperature 60～200 minutes, organic material is sunk in the collection section of quartzy tube assembly
Long-pending.
Preferably, described quartz tube assembly includes depth distillation groove, lead-over groove and the groove that slightly distils being sequentially connected in series, described depth
Degree distillation groove is located at the side near described first valve, and described thick distillation groove is located at the side near described second valve.
Preferably, the bidirectional vacuum sublimation purification equipment of described organic material also includes the sample-adding connecting with described lead-over groove
Groove, is provided with the 5th valve between described lead-over groove and described loading slot.
Preferably, described quartz tube assembly also includes be arranged between described depth distillation groove and described lead-over groove the 3rd
Valve, and it is arranged on the 4th valve between described lead-over groove and described thick distillation groove.
Preferably, the bidirectional vacuum sublimation purification equipment of described organic material also includes described quartz tube assembly is carried out adding
The heater of heat.
Present invention also offers a kind of continuous bidirectional vacuum sublimation purification method of organic material, comprise the steps：
1) organic material is placed in the lead-over groove of quartzy tube assembly and closes the 5th valve, close the first valve, the
Three valves, the 4th valve, and open the second valve, it is being evacuated to 10-3～10-4After Pa, open the 4th valve, to organic material
Material heated, temperature control 20～50 DEG C below the sublimation point of organic material, constant temperature 40～100 minutes, small molecule
Amount impurity is drawn in chiller.
2) close the second valve, open the first valve, the 3rd valve, organic material is heated, temperature control is having
More than the sublimation point of machine material between 0～80 DEG C, constant temperature 60～200 minutes, organic material is carried out in quartzy tube assembly
Distillation deposition, after the completion of distillation, adds new sample into lead-over groove by loading slot and closes the 5th valve.
3) repeat step 1) and step 2) n time, carry out continuous bidirectional vacuum sublimation purification, wherein, n >=1.
After completing continuous bidirectional vacuum distillation extraction, take out the organic material residues after the completion of distillation.
It is furthermore preferred that described chiller is the cold well of liquid nitrogen.
The bidirectional vacuum sublimation purification device structure of organic material provided by the present invention is simple, easily operated, efficient, has
Effect time-consuming in the case of improve organic material purity, continuous bidirectional vacuum sublimation purification can be carried out.
Brief description
Fig. 1 is the entirety of the bidirectional vacuum sublimation purification equipment of the organic material of first embodiment provided by the present invention
Structural representation.
Fig. 2 is the entirety of the bidirectional vacuum sublimation purification equipment of the organic material of second embodiment provided by the present invention
Structural representation.
In accompanying drawing 1,2, the list of parts representated by each label is as follows：
1st, vacuum cavity, 2, vacuum extractor, 3, quartzy tube assembly, 31, collection section, 32, bringing-up section, 33, depth distillation
Groove, 34, lead-over groove, 35, slightly distil groove, 36, loading slot, the 37, the 3rd valve, the 38, the 4th valve, the 39, the 5th valve, 4, first
Valve, the 5, second valve, 6, chiller, 7, heater.
Specific embodiment
Below in conjunction with accompanying drawing, the principle of the present invention and feature are described, illustrated embodiment is served only for explaining the present invention,
It is not intended to limit the scope of the present invention.
First embodiment
As shown in figure 1, a kind of bidirectional vacuum sublimation purification equipment of organic material, including：The circular tube shaped of both ends open
The vacuum cavity 1 of quartz material, vacuum extractor 2, chiller 6 and heater 7.Chiller 6 is the cold well of liquid nitrogen.Institute
The two ends stating vacuum cavity 1 are respectively arranged with the first valve 4 and the second valve 5, be provided with two ends and open in described vacuum cavity 1
The quartzy tube assembly 3 of mouth.Described quartz tube assembly 3 includes collection section 31 and the bringing-up section 32 connected.
Described vacuum extractor 2 is connected described chiller 6, and described chiller 6 is connected described first valve 4, described
Collection section 31 is located at the side near described first valve 4.
Described vacuum extractor 2 is connected described chiller 6, and described chiller 6 is connected described second valve 5, described
Bringing-up section 32 is located at the side near described second valve 5.
Heater 7 is arranged on the outside of vacuum cavity 1, for heat to bringing-up section 32.
The bidirectional vacuum sublimation purification method of organic material provided by the present invention is specific as follows：
1) organic material is placed in the bringing-up section 32 of quartzy tube assembly 3, closes the first valve 4 and open the second valve
5, it is being evacuated to 10-3～10-4After Pa, organic material is heated, temperature control is 20 below the sublimation point of organic material
～50 DEG C, constant temperature 40～100 minutes, small-molecular-weight impurity is drawn in chiller 6.
Under conditions of reaching fine vacuum, and less than sublimation point temperature 20-60 DEG C, the first valve is in closing shape
State, the second valve is in opening, and the impurity in organic material enters liquid nitrogen well by the second valve and is condensed deposition, when reaching
After certain time, the impurity in compound is removed.
2) close the second valve 5, open the first valve 4, organic material is heated, temperature control is in organic material
More than sublimation point between 0～80 DEG C, constant temperature 60～200 minutes, organic material enters in the collection section 31 of quartzy tube assembly 3
Row deposition.
Close the second valve, open the first valve, temperature is increased to above 10-100 DEG C of compound subliming point, so change
Compound will start to distil, and is deposited in the relatively low collection section of temperature, is high-purity compound that we need.
In the present embodiment, due to being provided with valve so that two ends shape in vacuum cavity at the two ends of vacuum cavity
Two two-way passages are become.By controlling the working condition of two valves and to the heating-up temperature of organic material so that one
Wing passage is used for the removal of small-molecular-weight impurity, and a wing passage is used for the collection of organic material, thus cleverly by small-molecular-weight
Impurity carries out separating in organic material, has reached the purpose of remove impurity purification.
Embodiment and effect example
It is distillation sample that the present embodiment adopts three (4- carbazole -9 bases-phenyl) amine (TCTA), and before distillation, sample purity is
96.8%, repeatedly distilled respectively, concrete operations flow process is as follows：
1) organic material is placed in the bringing-up section of quartz ampoule, closes the second valve and open the first valve, true taking out
Empty to 10-3～10-4After Pa, organic material is heated, temperature control 20 DEG C below the sublimation point of organic material, temperature
Continue 60 minutes, small-molecular-weight impurity is drawn in chiller.
2) close the first valve, open the second valve, continue organic material is heated, temperature control is in organic material
Sublimation point more than between 40 DEG C, constant temperature 120 minutes, organic material is deposited in the collection section of quartz ampoule.
3) complete to distil, close heater, be cooled to after room temperature after temperature, after vacuum breaker, collect the chemical combination of deposition section
Thing, and detect the purity of product.
Contrast on effect is carried out using the present invention and traditional equipment for purifying, the purity of its obtained product of two kinds of devices is as follows
Shown in table 1：
| Traditional method | This patent method | |
| Do not distil sample | 96.8% | 96.8% |
| Distil for the first time | 98.6% | 99.5% |
| Distil for second | 99.1% | 99.7% |
| Third time distils | 99.4% | 99.8% |
For organic material sublimation purification, if it is desired to the purity obtaining compound is higher, distillation difficulty is bigger, can from upper table
To find out, the two-way distillation that this patent is used, effectively achieve the separation of target compound and impurity, obtain higher pure
Degree.
Second embodiment
As shown in Fig. 2 a kind of bidirectional vacuum sublimation purification equipment of organic material, including：The circular tube shaped of both ends open
The vacuum cavity 1 of quartz material, vacuum extractor 2, chiller 6 and heater 7.Divide at the two ends of described vacuum cavity 1
It is not provided with the first valve 4 and the second valve 5, be provided with the quartzy tube assembly 3 of both ends open in described vacuum cavity 1.Institute
State depth distillation groove 33, lead-over groove 34 and the thick distillation groove 35 that quartzy tube assembly 3 includes being sequentially connected in series.In described depth distillation groove
It is provided with the 3rd valve 37 between 33 and described lead-over groove 34.It is provided between described lead-over groove 34 and described thick distillation groove 35
4th valve 38.
Described vacuum extractor 2 is connected described chiller 6, and described chiller 6 is connected described first valve 4, described
Depth distils groove 33 positioned at the side near described first valve 4.
Described vacuum extractor 2 is connected described chiller 6, and described chiller 6 is connected described second valve 5, described
Thick distillation groove 35 is located at the side near described second valve 5.
Heater 7 is arranged on the outside of vacuum cavity 1, for the depth distillation groove 33 to quartzy tube assembly 3 and slightly liter
Magnificent groove 35 etc. is heated.
For realizing continuous sublimation purification, the bidirectional vacuum sublimation purification equipment of described organic material also sets up and described mistake
The loading slot 36 of aqueduct 34 connection.Loading slot 36 can be communicated to the outside of vacuum cavity 1, realizes fast and easily continuous sample-adding.
It is provided with the 5th valve 39 between lead-over groove 34 and described loading slot 36.
The comprising the following steps that of the continuous bidirectional vacuum sublimation purification method of organic material provided by the present invention：
1) organic material is placed in the lead-over groove 34 of quartzy tube assembly 3 and closes the 5th valve 39, close the first valve
Door the 4, the 3rd valve 37, the 4th valve 38, and open the second valve 5, it is being evacuated to 10-3～10-4After Pa, open the 4th valve
Door 38, heats to organic material, temperature control 20～50 DEG C below the sublimation point of organic material, constant temperature 40～
100 minutes, small-molecular-weight impurity was drawn in chiller 6.
Under conditions of reaching fine vacuum, and less than sublimation point temperature 20-60 DEG C, the first valve is in closing shape
State, the second valve is in opening, and the impurity in organic material enters liquid nitrogen well by the second valve and is condensed deposition, when reaching
After certain time, the impurity in compound is by substantial amounts of removing.
After the completion of this step, the substantial amounts of material containing a small amount of impurity can be deposited on thick distillation groove 35.
2) close the second valve 5, open the first valve 4, the 3rd valve 37, organic material is heated, temperature control
More than the sublimation point of organic material between 0～80 DEG C, constant temperature 60～200 minutes, organic material enters in quartzy tube assembly 3
Row distillation deposition, after the completion of distillation, adds new sample into lead-over groove 34 by loading slot 36 and closes the 5th valve 39.
Close the second valve, open the first valve, the 3rd valve, temperature is increased to the above 10-100 of compound subliming point
DEG C, such compound will start to distil.During this, it is deposited on the less material of the thick impurity content distilling in groove 35
Material, in sublimation process this time, substantial amounts of depth of transferring to distils in groove 33, thus further increasing target compound
Purity.
3) repeat step 1) and step 2) repeatedly, carry out continuous bidirectional vacuum sublimation purification, take out remove impurity after the completion of purification
Organic material.
In step 1) and the repetitive process of step 2 in, the purity of organic material is through multiple in thick distillation groove 35 and deep
Degree distillation groove 33 back and forth in, impurity is constantly removed, thus further increasing the purity of target compound.
In the present embodiment, due to being provided with valve so that two ends shape in vacuum cavity at the two ends of vacuum cavity
Two two-way passages are become.By controlling the working condition of four valves and to the heating-up temperature of organic material so that one
Wing passage is used for the removal of small-molecular-weight impurity, and a wing passage is used for the collection of organic material.And, based on organic material thick
In the distillation repeatedly of distillation groove 35 and depth distillation groove 33, precipitation, by small-molecular-weight impurity in organic material maximum possible
Carry out separating, reached the purpose of remove impurity purification.
Embodiment and effect example
It is distillation sample that the present embodiment adopts three (4- carbazole -9 bases-phenyl) amine (TCTA), and before distillation, sample purity is
96.8%, repeatedly distilled respectively, concrete operations flow process is as follows：
1) organic material is placed in the lead-over groove of quartzy tube assembly and closes the 5th valve, close the first valve, the
Three valves, the 4th valve, and open the second valve, it is being evacuated to 10-3～10-4After Pa, open the 4th valve, to organic material
Material heated, temperature control 20 DEG C below the sublimation point of organic material, constant temperature 60 minutes, small-molecular-weight impurity is taken out
Enter in chiller, a large amount of sedimentation of organic material are in thick distillation groove.
2) close the second valve, open the first valve, the 3rd valve, organic material is heated, temperature control is having
More than the sublimation point of machine material between 40 DEG C, constant temperature 120 minutes, organic material is in the depth distillation groove of quartzy tube assembly
Deposited, after the completion of precipitation, new sample is added into lead-over groove by loading slot and closes the 5th valve；
3) new organic material, repeat step 3 times are added.
4) complete to distil, close heater, be cooled to after room temperature after temperature, after vacuum breaker, collect the chemical combination of deposition section
Thing, and detect the purity of product.
Contrast on effect is carried out using the present invention and traditional equipment for purifying, the purity of its obtained product of two kinds of devices is as follows
Shown in table 2：
| Traditional method | This patent method | |
| Do not distil sample | 96.8% | 96.8% |
| Distillation purity | 98.6% | 99.2% |
| Distillation amount | 200g | 600g |
For organic material sublimation purification, if it is desired to the purity obtaining compound is higher, distillation difficulty is bigger, can from upper table
To find out, the continuously two-way distillation that this patent is provided, effectively achieve the separation of target compound and impurity, obtain higher
Purity.With respect to common discontinuous vacuum sublimation, the distillation amount of target chemical combination is improved further.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of bidirectional vacuum sublimation purification equipment of organic material is it is characterised in that include vacuum cavity (1), vacuum means
Put (2) and chiller (6), be respectively arranged with the first valve (4) and the second valve (5) at the two ends of described vacuum cavity (1),
It is provided with the quartzy tube assembly (3) of both ends open in described vacuum cavity (1)；
Described vacuum extractor (2) the described chiller of series connection (6), described chiller (6) described first valve (4) of series connection,
One opening of described quartz tube assembly (3) is near described first valve (4)；
Described vacuum extractor (2) the described chiller of series connection (6), described chiller (6) described second valve (5) of series connection,
Another opening of described quartz tube assembly (3) near described second valve (5), wherein：
Described quartz tube assembly (3) includes collection section (31) and the bringing-up section (32) of series connection, and described collection section (31) is located at close
The side of described first valve (4), described bringing-up section (32) is located at the side near described second valve (5)；Or
Described quartz tube assembly (3) includes depth distillation groove (33), lead-over groove (34) and thick distillation groove (35) being sequentially connected in series, institute
State the depth groove (33) that distils and be located at side near described first valve (4), described thick distillation groove (35) is located near described the
The side of two valves (5).
2. organic material according to claim 1 bidirectional vacuum sublimation purification equipment it is characterised in that：Described organic material
The bidirectional vacuum sublimation purification equipment of material also includes the heater that described bringing-up section (32) is heated.
3. organic material according to claim 1 bidirectional vacuum sublimation purification equipment it is characterised in that：Described organic material
The bidirectional vacuum sublimation purification equipment of material also includes the loading slot (36) connecting with described lead-over groove (34), in described lead-over groove
(34) it is provided with the 5th valve (39) and described loading slot (36) between.
4. organic material according to claim 3 bidirectional vacuum sublimation purification equipment it is characterised in that：Described quartz ampoule
Assembly (3) also includes being arranged on the 3rd valve (37) that described depth distils between groove (33) and described lead-over groove (34), and
It is arranged on the 4th valve (38) between described lead-over groove (34) and described thick distillation groove (35).
5. organic material according to claim 4 bidirectional vacuum sublimation purification equipment it is characterised in that：Described organic material
The bidirectional vacuum sublimation purification equipment of material also includes the heater that described quartz tube assembly (3) is heated.
6. a kind of bidirectional vacuum sublimation purification method of organic material is it is characterised in that organic material according to claim 2
The bidirectional vacuum sublimation purification equipment of material, is carried out including the steps：
1) organic material is placed in the bringing-up section (32) of quartzy tube assembly (3), closes the first valve (4) and open the second valve
Door (5), is being evacuated to 10-3～10-4After Pa, organic material is heated, temperature control organic material sublimation point with
Lower 20～50 DEG C, constant temperature 40～100 minutes, small-molecular-weight impurity is drawn in chiller (6)；
2) close the second valve (5), open the first valve (4), organic material is heated, temperature control is in organic material
More than sublimation point between 0～80 DEG C, constant temperature 60～200 minutes, organic material is in the collection section (31) of quartzy tube assembly (3)
In deposited.
7. a kind of continuous bidirectional vacuum sublimation purification method of organic material is it is characterised in that according to claim 5 have
The bidirectional vacuum sublimation purification equipment of machine material, is carried out including the steps：
1) organic material is placed in the lead-over groove (34) of quartzy tube assembly (3) and cuts out the 5th valve (39), close first
Valve (4), the 3rd valve (37), the 4th valve (38), and open the second valve (5), it is being evacuated to 10-3～10-4After Pa,
Open the 4th valve (38), organic material is heated, temperature control is 20～50 DEG C below the sublimation point of organic material, warm
Degree continues 40～100 minutes, and small-molecular-weight impurity is drawn in chiller (6)；
2) close the second valve (5), open the first valve (4), the 3rd valve (37), organic material is heated, temperature control
Make more than the sublimation point of organic material between 0～80 DEG C, constant temperature 60～200 minutes, organic material is in quartzy tube assembly
(3) carry out distillation deposition, after the completion of distillation, new sample is added into lead-over groove (34) by loading slot (36) and closes the 5th
Valve (39)；
3) repeat step 1) and step 2) n time, carry out continuous bidirectional vacuum sublimation purification, wherein, n >=1.
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| CN108992962B (en) * | 2018-09-30 | 2024-05-31 | 深圳普瑞材料技术有限公司 | Modularized sublimation purification system |
| US20200165270A1 (en) * | 2018-11-28 | 2020-05-28 | Versum Materials Us, Llc | Low Halide Lanthanum Precursors For Vapor Deposition |
| CN109499090A (en) * | 2018-12-25 | 2019-03-22 | 威格气体纯化科技（苏州）股份有限公司 | A kind of apophorometer with control material processing environmental functional |
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| CN101738062B (en) * | 2008-11-14 | 2012-09-19 | 兰州科近真空冻干技术有限公司 | Vacuum freeze-drying device |
| CN102671411B (en) * | 2012-05-16 | 2015-01-14 | 六盘水神驰生物科技有限公司 | Device for recovering pyrogallic acids through electrostatic adsorption by using sublimation method |
| CN204601665U (en) * | 2015-01-29 | 2015-09-02 | 武汉尚赛光电科技有限公司 | Continuous or the discontinuous bidirectional vacuum sublimation purification equipment of organic material |
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Application publication date: 20150603 Assignee: HUBEI SUNSHINE OPTOELECTRONICS MATERIAL CO.,LTD. Assignor: WUHAN SUNSHINE OPTOELECTRONICS TECH Co.,Ltd. Contract record no.: 2017420000003 Denomination of invention: Organic material bi-directional vacuum sublimation purification equipment and continuous or non-continuous purifying method Granted publication date: 20170222 License type: Exclusive License Record date: 20170317 |
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Denomination of invention: Organic material bi-directional vacuum sublimation purification equipment and continuous or non-continuous purifying method Effective date of registration: 20200521 Granted publication date: 20170222 Pledgee: Hubei Guo Chuang financing Company limited by guarantee Pledgor: WUHAN SUNSHINE OPTOELECTRONICS TECH Co.,Ltd. Registration number: Y2020420000020 |
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