CN102961890B - Equipment and process for vacuum sublimation purification of small organic molecule material - Google Patents
Equipment and process for vacuum sublimation purification of small organic molecule material Download PDFInfo
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- CN102961890B CN102961890B CN201210535651.1A CN201210535651A CN102961890B CN 102961890 B CN102961890 B CN 102961890B CN 201210535651 A CN201210535651 A CN 201210535651A CN 102961890 B CN102961890 B CN 102961890B
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Abstract
The invention provides equipment for vacuum sublimation purification of a small organic molecule material. The equipment comprises a quartz sublimation pipe, a vacuumizing device for vacuumizing the quartz sublimation pipe, a film thickness detector and a heating device, wherein the film thickness detector is capable of detecting the diffusion rate of the small organic molecule material after sublimation in the quart sublimation pipe and comprises a probe capable of contacting small organic molecules, and a signal processor which is connected with the probe and used for sending out a diffusion rate signal; and the heating device is used for heating each temperature zone of the quartz sublimation pipe and adjusting according to the diffusion rate. The equipment provided by the invention realizes effective control on the vacuum sublimation purification process of the small organic molecule material, and further realizes reduction of pollution and waste while improving the purification speed and the purity and quality of the material. The invention also provides a process for the vacuum sublimation purification of the small organic molecule material, which is implemented by the equipment for the vacuum sublimation purification of the small organic molecule material provided by the invention.
Description
Technical field
The present invention relates to highly purified organic photoelectrical material manufacturing technology field, more particularly, relate to the equipment that a kind of organic small molecule material vacuum sublimation is purified, the invention still further relates to the technique that a kind of organic small molecule material vacuum sublimation is purified.
Background technology
In order to meet the demand of organic electro-optic device field to material, China's organic photoelectrical material industry need to produce high-quality, highly purified organic photoelectrical material, could obtain high performance organic electro-optic device.
Prior art often adopts vacuum sublimation technology to purify to organic small molecule material.The vacuum sublimation equipment for purifying using at present adopts the design of three sections of temperature controls or five sections of temperature controls, obtain high vacuum atmosphere by the coupling of mechanical pump, molecular pump, then respectively different warm areas are regulated and controled, utilize the different sublimation temperatures of different component material to come separating-purifying acquisition high-quality, highly purified organic small molecule material.
Existing vacuum sublimation equipment for purifying, by regulating the heating-up temperature of heater, is controlled the diffusion rate after organic small molecule material distillation.But, the experience that often depends on technical staff in concrete operations regulates heater with sensation, lack the effective monitoring to purification process, can not realize the effective control to organic small molecule material vacuum sublimation purification process, be not easy to control the diffusion rate of organic molecule; So that hour affect purifying velocity when diffusion rate, and then affect production efficiency; In the time that diffusion rate is larger, organic molecule can be diffused into again in vavuum pump, and vavuum pump is caused to serious pollution, and can cause the waste of material.Meanwhile, due to effective control that can not realize organic small molecule material vacuum sublimation purification process, cause purity and the inferior quality of material.
In sum, the equipment that how to provide a kind of organic small molecule material vacuum sublimation to purify, to realize the effective control to organic small molecule material vacuum sublimation purification process, and then realize in improving the purity of purifying velocity and material and quality and reduce and pollute and waste, be current those skilled in the art technical problems urgently to be resolved hurrily.
Summary of the invention
In view of this, the equipment that the object of the present invention is to provide a kind of organic small molecule material vacuum sublimation to purify, to realize effective control to organic small molecule material vacuum sublimation purification process, and then realize in improving the purity of purifying velocity and material and quality and reduce and pollute and waste.
The technique that the present invention also provides a kind of organic small molecule material vacuum sublimation to purify, its equipment of applying organic small molecule material vacuum sublimation purification provided by the invention carries out.
In order to achieve the above object, the invention provides following technical scheme:
The equipment that organic small molecule material vacuum sublimation is purified, comprises quartzy sublimation pipe and the vacuum extractor for described quartzy sublimation pipe is vacuumized; Also comprise:
The thickness detector of the diffusion rate after the organic small molecule material distillation in described quartzy sublimation pipe can be detected, described thickness detector comprise can with the organic molecule probe that contact after distillation be connected with described probe, and send the signal processor of diffusion rate signal;
For the each section of heater that warm area heats to described quartzy sublimation pipe;
Receive described diffusion rate signal, for controlling the regulation device of described heater, it regulates control according to received diffusion rate signal to described heater, in the time that described diffusion rate is less than the rate of sublimation critical value of setting, make described heater continue the temperature of the described each section of warm area of rising; In the time that described diffusion rate equals described rate of sublimation critical value, make described heater keep the temperature constant of described each section of warm area; In the time that described diffusion rate is greater than described rate of sublimation critical value, make described heater reduce the temperature of described each section of warm area.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, described regulation device is to be connected with described heater, receive the first controller of described diffusion rate signal, described the first controller is made comparisons described diffusion rate and described rate of sublimation critical value, in the time that described diffusion rate is less than described rate of sublimation critical value, control described heater persistently overheating; In the time that described diffusion rate equals described rate of sublimation critical value, control described heater and keep temperature constant; In the time that described diffusion rate is greater than described rate of sublimation critical value, controls described heater and reduce temperature.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, also comprise:
By the manual regulating device of heater described in manual adjustments control; With
The switching device shifter being connected with described manual regulating device with described the first controller respectively.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, described probe is arranged on one end near outlet in described quartzy sublimation pipe.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, described vacuum extractor comprises:
Mechanical pump, the air entry of described mechanical pump is connected with described quartzy sublimation pipe by the first pipeline, and on described the first pipeline, is provided with mechanical pump and takes out in advance valve;
Molecular pump, the air entry of described molecular pump is connected with described quartzy sublimation pipe by the second pipeline, and exhaust outlet is connected with the air entry of described mechanical pump, and is provided with molecular pump valve on described the second pipeline.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, also comprise:
Be arranged on described quartzy sublimation pipe, for measuring the concurrent vacuum meter that send air pressure signal of air pressure in described quartzy sublimation pipe;
Be connected with described vacuum meter, receive the second controller of described air pressure signal, in the time that the air pressure in described quartzy sublimation pipe is greater than 50Pa, controls described mechanical pump and take out in advance valve and open, in the time that described air pressure is less than or equal to 50Pa, controls described mechanical pump and take out in advance valve and close;
Be connected with described vacuum meter, receive the 3rd controller of described air pressure signal, in the time that described air pressure is less than or equal to 50Pa, control described molecular pump and described molecular pump valve opening simultaneously;
Be connected with described vacuum meter, receive the 4th controller of described air pressure signal, in the time that described air pressure reaches the vacuum of setting, control described heater and open.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, the suction opeing of described the first pipeline is connected with described the second pipeline between described molecular pump valve and described quartzy sublimation pipe.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, described the second pipeline is connected by screwed flange with described quartzy sublimation pipe, and coordinates by seal with elastometic washer.
Preferably, in the equipment that above-mentioned organic small molecule material vacuum sublimation is purified, described quartzy sublimation pipe is the cylindrical quartz pipe obtaining by artificial drawing, an end opening of described cylindrical quartz pipe, other end sealing.
Can find out from above-mentioned technical scheme, the equipment that organic small molecule material vacuum sublimation provided by the invention is purified, in the process of purifying, first vacuumizes quartzy sublimation pipe by vacuum extractor; Then opening heater heats each section of warm area of quartzy sublimation pipe; And then the organic small molecule material in quartzy sublimation pipe is distilled under vacuum environment, the organic small molecule material after distillation can spread; After organic molecule contacts with the probe of thickness detector, probe can send the signal of its detection to signal processor, and this signal processor is converted to the diffusion rate after organic small molecule material distillation by signal; Then regulation device is made comparisons the rate of sublimation critical value of above-mentioned diffusion rate and setting, regulates heater according to diffusion rate, and the rate of sublimation critical value of this setting is the maximal sublimation rate that can not be diffused into quartzy sublimation pipe outside; In the time that diffusion rate is less than rate of sublimation critical value, make heater continue the temperature of each section of warm area of rising; In the time that diffusion rate equals rate of sublimation critical value, make heater keep the temperature constant of each section of warm area; In the time that diffusion rate is greater than rate of sublimation critical value, make heater reduce the temperature of each section of warm area; Make diffusion rate after organic small molecule material distillation finally maintain the rate of sublimation critical value of setting by above regulation and control.
In summary, the equipment that organic small molecule material vacuum sublimation provided by the invention is purified is in the process of purifying, detect and obtain the diffusion rate after organic small molecule material distillation by thickness detector, realize the effective monitoring to purification process, and utilize regulation device reasonably to regulate heater to realize the demand of different temperatures according to above-mentioned diffusion rate, make diffusion rate finally maintain the rate of sublimation critical value of setting; Therefore the equipment that organic small molecule material vacuum sublimation provided by the invention is purified has been avoided affecting purifying velocity or the excessive organic molecule that causes of diffusion rate is diffused into the phenomenon in vavuum pump because of diffusion rate compared with little, realize the effective control to organic small molecule material vacuum sublimation purification process, and then realized in improving the purity of purifying velocity and material and quality and reduced and pollute and waste.
The technique that the present invention also provides a kind of organic small molecule material vacuum sublimation to purify, the equipment that the organic small molecule material vacuum sublimation that the above-mentioned any one technical scheme of its utilization the present invention provides is purified carries out, and comprises step:
1) vacuumize: utilize described vacuum extractor to vacuumize described quartzy sublimation pipe, and the air pressure in described quartzy sublimation pipe is measured simultaneously;
2) open described heater: in the time that the air pressure in described quartzy sublimation pipe reaches the vacuum of setting, open described heater, it is heated each section of warm area of described quartzy sublimation pipe;
3) utilize described thickness detector to detect the diffusion rate after the organic small molecule material distillation in described quartzy sublimation pipe, and according to described diffusion rate, described heater is regulated, make described diffusion rate finally maintain the rate of sublimation critical value of setting:
In the time that described diffusion rate is less than the rate of sublimation critical value of setting, make described heater continue the temperature of the described each section of warm area of rising; In the time that described diffusion rate equals described rate of sublimation critical value, make described heater keep the temperature constant of described each section of warm area; In the time that described diffusion rate is greater than described rate of sublimation critical value, make described heater reduce the temperature of described each section of warm area.
Preferably, in the technique that above-mentioned organic small molecule material vacuum sublimation is purified, described step 1) be specially:
11) open the mechanical pump of described vacuum extractor, utilize described in second controller control the mechanical pump of vacuum extractor to take out in advance valve and open, described mechanical pump is vacuumized described quartzy sublimation pipe;
12) by vacuum meter, the air pressure in described quartzy sublimation pipe is measured, in the time that described air pressure is less than or equal to 50Pa, utilizing described in second controller control mechanical pump to take out in advance valve closes, the molecular pump and the molecular pump valve opening that utilize vacuum extractor described in the 3rd controller control link up described molecular pump and described mechanical pump described quartzy sublimation pipe are vacuumized simultaneously;
Described step 2) be specially:
Open by heater described in the 4th controller control, described heater is resistive heating device;
Described step 3) specifically by the first controller, described heater is regulated, in the time that described diffusion rate is less than described rate of sublimation critical value, heater is persistently overheating described in described the first controller control; In the time that described diffusion rate equals described rate of sublimation critical value, heater keeps temperature constant described in described the first controller control; In the time that described diffusion rate is greater than described rate of sublimation critical value, heater reduces temperature described in described the first controller control.
Can find out from above-mentioned technical scheme, the technology utilization thickness detector that organic small molecule material vacuum sublimation provided by the invention is purified detects the diffusion rate after the organic small molecule material distillation in quartzy sublimation pipe, realize the effective monitoring to purification process, and reasonably regulate heater to realize the demand of different temperatures according to above-mentioned diffusion rate, make diffusion rate finally maintain the rate of sublimation critical value of setting; Therefore the technique that organic small molecule material vacuum sublimation provided by the invention is purified has been avoided affecting purifying velocity or diffusion rate causes more greatly organic molecule to be diffused into the phenomenon in vavuum pump because of diffusion rate compared with little, realize the effective control to organic small molecule material vacuum sublimation purification process, and then realized in improving the purity of purifying velocity and material and quality and reduced and pollute and waste.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of the organic small molecule material vacuum sublimation that provides of the embodiment of the present invention equipment of purifying;
Fig. 2 is the process flow diagram of the organic small molecule material vacuum sublimation that provides of the embodiment of the present invention technique of purifying.
Detailed description of the invention
The equipment that the embodiment of the present invention provides a kind of organic small molecule material vacuum sublimation to purify, realize the effective control to organic small molecule material vacuum sublimation purification process, and then realized in improving the purity of purifying velocity and material and quality and reduced and pollute and waste.
For making object, technical scheme and the advantage of the embodiment of the present invention clearer, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Please refer to accompanying drawing 1, the equipment that the organic small molecule material vacuum sublimation that the embodiment of the present invention provides is purified, comprises quartzy sublimation pipe 1, vacuum extractor, heater 11, regulation device and thickness detector 2, wherein, vacuum extractor is for vacuumizing quartzy sublimation pipe 1; Thickness detector 2 can detect the diffusion rate after the distillation of organic small molecule material in quartzy sublimation pipe 1, and it comprises that the probe 21 that can contact with the organic molecule after distillation 21 is connected with popping one's head in, and sends the signal processor 22 of diffusion rate signal; Heater 11 heats for the each section of warm area to quartzy sublimation pipe 1; Regulation device receives diffusion rate signal, for controlling heater 11, it regulates control according to received diffusion rate signal to heater 11, in the time that diffusion rate is less than the rate of sublimation critical value of setting, make heater 11 continue the temperature of each section of warm area of rising; In the time that diffusion rate equals rate of sublimation critical value, make heater 11 keep the temperature constant of each section of warm area; In the time that diffusion rate is greater than rate of sublimation critical value, make heater 11 reduce the temperature of each section of warm area.
It should be noted that, probe 21 in thickness detector 2 is quartz wafers, organic molecule after distillation can be met the cold surface that condenses in quartz wafer after being diffused into probe 21 position, increase the weight of quartz wafer, then pop one's head in and 21 send the weight signal of the quartz wafer of its detection to signal processor 22, signal processor 22 utilizes the intrinsic frequency of crystal and the quality of crystal this law that is inversely proportional to, and can obtain the diffusion rate after organic small molecule material distillation according to the changing down of quartz wafer intrinsic frequency by signal conversion.
The concrete mode that adopts three sections of temperature controls of the embodiment of the present invention is carried out subliming purification process, as shown in Figure 1, each section of warm area of the quartzy sublimation pipe 1 of the present embodiment specifically comprises three sections of warm areas that heat by heater 11 respectively: be arranged on the first warm area A of exporting near quartzy sublimation pipe 1, at the three-temperature-zone C of quartzy sublimation pipe 1 bottom and be arranged on the second warm area B between the first warm area A and three-temperature-zone C, and the temperature of three-temperature-zone C, the second warm area B and the first warm area A reduces successively, so that three warm area formation temperature gradients.Three-temperature-zone C is the position that organic small molecule material sample is initially laid, after heating apparatus 11 heats three warm areas, the temperature of three-temperature-zone C is the highest, in the time that temperature reaches certain value, the organic small molecule material that is positioned at three-temperature-zone C will be sublimed into the organic molecule of gaseous state, organic molecule can be in quartzy sublimation pipe 1 diffusion inside, is then diffused into condensation after the second warm area B and the first warm area A, and then realizes and purifying.Be understandable that, the present embodiment is not limited to the arrangement of above-mentioned heating region, can also adopt the mode of five sections or other section of temperature control to carry out subliming purification process.
The equipment that the organic small molecule material vacuum sublimation that the embodiment of the present invention provides is purified, in the process of purifying, first vacuumizes quartzy sublimation pipe 1 by vacuum extractor; Then opening heater 11 heats 1 each section of warm area of quartzy sublimation pipe; And then the organic small molecule material in quartzy sublimation pipe 1 is distilled under vacuum environment, the organic small molecule material after distillation can spread; After organic molecule contacts with the probe 21 of thickness detector 2, probe 21 can send the signal of its detection to signal processor 22, and this signal processor 22 is converted to the diffusion rate after organic small molecule material distillation by signal; Then utilize regulation device that the rate of sublimation critical value of above-mentioned diffusion rate and setting is made comparisons, regulate heater 11 according to diffusion rate, the rate of sublimation critical value of this setting is the maximal sublimation rate that can not be diffused into quartzy sublimation pipe 1 outside; In the time that diffusion rate is less than rate of sublimation critical value, make heater 11 continue the temperature of rising the first warm area A, the second warm area B and three-temperature-zone C; In the time that diffusion rate equals rate of sublimation critical value, make heater 11 keep the temperature constant of the first warm area A, the second warm area B and three-temperature-zone C; In the time that diffusion rate is greater than rate of sublimation critical value, make heater 11 reduce the temperature of three-temperature-zone C, to realize the diffusion rate of the organic molecule material that reduces C place, three-temperature-zone; Make diffusion rate after organic small molecule material distillation finally maintain the rate of sublimation critical value of setting by above regulation and control.
In summary, the equipment that the organic small molecule material vacuum sublimation that the embodiment of the present invention provides is purified is in the process of purifying, detect and obtain the diffusion rate after organic small molecule material distillation by thickness detector 2, realize the effective monitoring to purification process, and reasonably regulate heater 11 to realize the demand of different temperatures according to above-mentioned diffusion rate, make diffusion rate finally maintain the rate of sublimation critical value of setting; Therefore the equipment that the organic small molecule material vacuum sublimation that the embodiment of the present invention provides is purified has been avoided affecting purifying velocity or the excessive organic molecule that causes of diffusion rate is diffused into the phenomenon in vavuum pump because of diffusion rate compared with little, realize the effective control to organic small molecule material vacuum sublimation purification process, and then realized in improving the purity of purifying velocity and material and quality and reduced and pollute and waste.
In addition, the present embodiment has been realized the effective monitoring to purification process by having increased thickness detector 2, and monitoring method is simple and cost is lower.Meanwhile, the embodiment of the present invention can be set different rate of sublimation critical values according to different organic molecule materials, reduced pollution in purification process and the waste of material, has expanded the range of application of the equipment that vacuum sublimation purifies simultaneously.
Preferably, in the equipment that the organic small molecule material vacuum sublimation that above-described embodiment provides is purified, regulation device is to be connected with heater 11, receive the first controller of diffusion rate signal, the first controller is made comparisons diffusion rate and rate of sublimation critical value, in the time that diffusion rate is less than rate of sublimation critical value, control the heating power of heater 11 with the temperature of raise the first warm area A, the second warm area B and three-temperature-zone C; In the time that diffusion rate equals rate of sublimation critical value, control the heating power of heater 11 to keep the temperature constant of the first warm area A, the second warm area B and three-temperature-zone C; In the time that diffusion rate is greater than rate of sublimation critical value, the heating power of controlling heater 11 reduces the temperature of three-temperature-zone C.
In the process that the equipment that above-mentioned organic small molecule material vacuum sublimation is purified is purified, detect the diffusion rate after the organic small molecule material distillation in quartzy sublimation pipe 1 by thickness detector 2, and send diffusion rate signal; Utilize the first controller to receive diffusion rate signal, and by above-mentioned diffusion rate and the comparison of rate of sublimation critical value, and then regulate heater 11 according to different situations, in the time that diffusion rate is less than rate of sublimation critical value, utilize the heating power of the first controller control heater 11 with the temperature of raise the first warm area A, the second warm area B and three-temperature-zone C; In the time that diffusion rate equals rate of sublimation critical value, utilize the heating power of the first controller control heater 11 to keep the temperature constant of the first warm area A, the second warm area B and three-temperature-zone C; In the time that diffusion rate is greater than rate of sublimation critical value, utilize the heating power of the first controller control heater 11 to reduce the temperature of three-temperature-zone C.Make diffusion rate after organic small molecule material distillation finally maintain the rate of sublimation critical value of setting by above regulation and control.
From the above mentioned, the present embodiment utilizes the first controller to receive diffusion rate signal, and then the heating power of controlling heater 11 is to adjust the temperature of different warm areas, realize the automatic control to heater, and then realize the precision control to organic small molecule material vacuum sublimation purification process, further improve the vacuum sublimation purification efficiency of purity and quality and the organic small molecule material of material, reduced the input of manpower simultaneously.It will be understood by those skilled in the art that, this heater 11 also can be by manual control, operating personnel are by making comparisons the rate of sublimation critical value of the diffusion rate of obtaining and setting, and then the heating power of heater 11 is regulated, to reach the same effect that makes diffusion rate after organic small molecule material distillation finally maintain the rate of sublimation critical value of setting.
In order further to optimize technique scheme, in the equipment that the organic small molecule material vacuum sublimation that above-described embodiment provides is purified, also comprise by the manual regulating device of manual adjustments control heater 11 and the switching device shifter being connected with manual regulating device with the first controller respectively.Now, the equipment that the vacuum sublimation of the present embodiment is purified has manual work pattern and automatic operation mode, and switching device shifter can be realized the switching between manual work pattern and the automatic operation mode of the equipment that vacuum sublimation purifies.When switching device shifter is opened the first controller, while closing manual regulating device, the equipment that the vacuum sublimation of the present embodiment is purified is in automatic operation mode, realize automatic adjusting heater 11, and then realized the diffusion rate making in the short period of time after organic small molecule material distillation and maintain the rate of sublimation critical value of setting.When switching device shifter cuts out the first controller, while opening manual regulating device, the equipment that the vacuum sublimation of the present embodiment is purified is in manual work pattern, and the equipment that convenient operation personnel purify to vacuum sublimation in time as required in distillation purification process is made and revised and adjust.
Concrete, in the equipment that the organic small molecule material vacuum sublimation that above-described embodiment provides is purified, probe 21 is arranged on the interior one end near outlet of quartzy sublimation pipe 1.Because probe 21 is arranged in quartzy sublimation pipe 1, be convenient to the organic small molecule material after distillation to contact with the probe 21 of thickness detector 2, and then be convenient to the transmission of signal, improve the accuracy of surveying.Simultaneously, due to probe 21 outlets near quartzy sublimation pipe 1, just can detect so only have when organic small molecule material is diffused into exit probe 21, be that the diffusion rate of organic molecule and range of scatter just can detect when enough large, can shorten the regulation and control time of heater 11, improve purification rate.Certainly, probe 21 also can be arranged on quartzy sublimation pipe 1 and be connected, and near in the vacuum cavity of quartzy sublimation pipe 1, to realize equally the object of the organic small molecule material that can detect diffusion.
Preferably, in the equipment that the organic small molecule material vacuum sublimation that above-described embodiment provides is purified, vacuum extractor comprises mechanical pump 5 and molecular pump 9, wherein, the air entry of mechanical pump 5 is connected with quartzy sublimation pipe 1 by the first pipeline 6, and on the first pipeline 6, is provided with mechanical pump and takes out in advance valve 4; The air entry of molecular pump 9 is connected with quartzy sublimation pipe 1 by the second pipeline 7, and exhaust outlet is connected with the air entry of mechanical pump 5, and is provided with molecular pump valve 8 on the second pipeline 7.
Concrete, the mechanical pump 5 in the present embodiment is the vacuum mechanical pump of at least four liters of pumping speed, this vacuum mechanical pump can ensure the speed vacuumizing, and has heat dispersion preferably simultaneously, has extended the duration of runs, has improved the service life of vacuum extractor.Mechanical pump is taken out in advance valve 4 and is adopted common vacuum needle-valve or reset valve, can critically control the speed vacuumizing of mechanical pump 5.Molecular pump 9 adopts power to be not less than the vacuum molecular pump of 600 watts, and when its work and mechanical pump 5 be serially connected, ensured to have improved the speed that vacuumizes and vacuumized efficiency.Molecular pump valve 8 adopts slide valve equal vacuum control valve.
The vacuum of above-mentioned vacuum extractor is as follows:
First opening mechanical pump 5 and mechanical pump takes out in advance valve 4 and opens, now the first pipeline 6 is path, utilizes mechanical pump 5 to vacuumize quartzy sublimation pipe 1, has realized taking out in advance quartzy sublimation pipe 1, reduce the force value in quartzy sublimation pipe 1, reduced the damage to its blade while opening molecular pump 9; In the time that the pressure in quartzy sublimation pipe 1 drops to certain value, close mechanical pump and take out in advance valve 4, in the present embodiment, specifically this value is made as to 50Pa, can reduce the blade of molecular pump 9 is damaged, the pump oil that can reduce again mechanical pump 5 is diffused into the pollution causing in vacuum environment; Open successively molecular pump 9 and molecular pump valve 8, now the second pipeline 7 is path, and the air entry of mechanical pump 5 is connected with the exhaust outlet of molecular pump 9, mechanical pump 5 is as the fore pump of molecular pump 9, coupling by mechanical pump 5 and molecular pump 9 vacuumizes quartzy sublimation pipe 1, so that the higher vacuum of the interior acquisition of quartzy sublimation pipe 1, thereby be conducive to the diffusion of gaseous state organic small molecule material, reduced pollution and loss to material simultaneously.
Further, in the equipment that the organic small molecule material vacuum sublimation that above-described embodiment provides is purified, also comprise:
Be arranged on quartzy sublimation pipe 1, for measuring the concurrent vacuum meter 3 that send air pressure signal of air pressure in quartzy sublimation pipe 1;
Be connected with vacuum meter 3, receive the second controller of air pressure signal, in the time that the air pressure in quartzy sublimation pipe 1 is greater than 50Pa, control mechanical pump is taken out in advance valve 4 and is opened, and in the time that air pressure is less than or equal to 50Pa, control mechanical pump is taken out in advance valve 4 and closed;
Be connected with vacuum meter 3, receive the 3rd controller of air pressure signal, in the time that air pressure is less than or equal to 50Pa, control molecular pump 9 and molecular pump valve 8 is opened simultaneously;
Be connected with vacuum meter 3, receive the 4th controller of air pressure signal, in the time that air pressure reaches the vacuum of setting, control heater and open.
In the equipment that above-mentioned vacuum sublimation is purified; the keying of taking out in advance valve 4 by second controller control mechanical pump respectively; open by the 3rd controller control molecular pump 9 and molecular pump valve 8; open by the 4th controller control heater 11; and regulate heater 11 by the first controller; realize full-automatic operation, can realize the production of scale.
For the ease of the installation of pipeline, the suction opeing of above-mentioned the first pipeline 6 is connected with the second pipeline 7 between molecular pump valve 8 and quartzy sublimation pipe 1.As shown in Figure 1, the suction opeing of the first pipeline 6 is connected with the second pipeline 7 respectively with the mouth of the air entry of mechanical pump 5 near the mouth of quartzy sublimation pipe 1 and air outlet, like this, 1 of sublimation pipe of quartz need to be connected with one end of the second pipeline 7, the two ends of the first pipeline 6 are separately positioned on the two ends of the second pipeline 7, install simply, and be convenient to the sealing to quartzy sublimation pipe 1.Certainly, the first pipeline 6 can also directly be connected with quartzy sublimation pipe 1.
Preferably, the second pipeline 7 is connected by screwed flange with quartzy sublimation pipe 1, and coordinates by seal with elastometic washer.By screwed flange, the second pipeline 7 is connected with quartzy sublimation pipe 1, be convenient to the installation and removal of quartzy sublimation pipe 1, use seal with elastometic washer to make both junctions there is good sealing effectiveness, and then ensure that quartzy sublimation pipe 1 inside can obtain higher vacuum; Meanwhile, rubber ring has the effect of damping, buffering, has reduced the chipping phenomenon of quartzy sublimation pipe 1.
Concrete, the cylindrical quartz pipe of above-mentioned quartzy sublimation pipe 1 for obtaining by artificial drawing, an end opening of this cylindrical quartz pipe, other end sealing.While using this cylindrical quartz pipe, organic small molecule material is laid in one end of sealing to the bottom of pipe by opening, when pending purification, this opening is sealed and is connected by flange seal or with the second pipeline 7.Because the inwall of cylindrical pipe seamlessly transits, there is no dead angle, be convenient to the diffusion of organic small molecule material, improve purity and the quality of material.
Please refer to accompanying drawing 2, the technique that the embodiment of the present invention also provides a kind of organic small molecule material vacuum sublimation to purify, the equipment that the organic small molecule material vacuum sublimation that its utilization embodiment of the present invention any one provides is purified carries out, and comprises step:
S1: vacuumize:
Utilize vacuum extractor to vacuumize quartzy sublimation pipe 1, and the air pressure in quartzy sublimation pipe 1 is measured simultaneously;
S2: open heater 11:
In the time that the air pressure in quartzy sublimation pipe 1 reaches the vacuum of setting, open heater 11, it is heated 1 each section of warm area of quartzy sublimation pipe, in concrete the present embodiment, respectively the first warm area A, the second warm area B and three-temperature-zone C are heated;
S3: utilize thickness detector 2 to detect the diffusion rate after the organic small molecule material distillation in quartzy sublimation pipe 1, and according to above-mentioned diffusion rate, heater 11 is regulated, make diffusion rate finally maintain the rate of sublimation critical value of setting:
In the time that diffusion rate is less than the rate of sublimation critical value of setting, make heater 11 continue the temperature of each section of warm area of rising; In the time that diffusion rate equals rate of sublimation critical value, make heater 11 keep the temperature constant of each section of warm area; In the time that diffusion rate is greater than rate of sublimation critical value, make heater 11 reduce the temperature of each section of warm area.
The technology utilization thickness detector 2 that the organic small molecule material vacuum sublimation that the embodiment of the present invention provides is purified detects the diffusion rate after the organic small molecule material distillation in quartzy sublimation pipe 1, realize the effective monitoring to purification process, and reasonably regulate heater 11 to realize the demand of different temperatures according to above-mentioned diffusion rate, make diffusion rate finally maintain the rate of sublimation critical value of setting; Therefore the technique that the organic small molecule material vacuum sublimation that the embodiment of the present invention provides is purified has been avoided affecting purifying velocity or the excessive organic molecule that causes of diffusion rate is diffused into the phenomenon in vavuum pump because of diffusion rate compared with little, realize the effective control to organic small molecule material vacuum sublimation purification process, and then realized in improving the purity of purifying velocity and material and quality and reduced and pollute and waste.
Preferably, in the technique that the organic small molecule material vacuum sublimation that above-described embodiment provides is purified, step S1 is specially:
S11: open the mechanical pump 5 of vacuum extractor, utilize the mechanical pump of second controller control vacuum extractor to take out in advance valve 4 and open, mechanical pump 5 is vacuumized quartzy sublimation pipe 1;
Realize the taking out in advance of quartzy sublimation pipe 1 by mechanical pump 5, reduced the force value in quartzy sublimation pipe 1, reduced the damage to its blade while opening molecular pump 9; In the time that the pressure in quartzy sublimation pipe 1 drops to certain value, close mechanical pump and take out in advance valve 4, in the present embodiment, specifically this value is made as to 50Pa, can reduce the blade of molecular pump 9 is damaged, the pump oil that can reduce again mechanical pump 5 is diffused into the pollution causing in vacuum environment;
S12: the air pressure in quartzy sublimation pipe 1 is measured by vacuum meter 3, in the time that air pressure is less than or equal to 50Pa, utilizing second controller control mechanical pump to take out in advance valve 4 closes, utilize molecular pump 9 and the molecular pump valve 8 of the 3rd controller control vacuum extractor to open simultaneously, molecular pump 9 and mechanical pump 5 are linked up quartzy sublimation pipe 1 is vacuumized;
Coupling by mechanical pump 5 and molecular pump 9 vacuumizes quartzy sublimation pipe 1, so that the higher vacuum of the interior acquisition of quartzy sublimation pipe 1, thereby is conducive to the diffusion of gaseous state organic small molecule material, has reduced pollution and loss to material simultaneously.
Step S2 is specially:
Open by the 4th controller control heater 11, heater 11 is preferably resistive heating device, adopts resistance heated mode fairly simple, has reduced input cost;
Step S3 specifically regulates heater 11 by the first controller, and in the time that diffusion rate is less than rate of sublimation critical value, the first controller control heater 11 is persistently overheating; In the time that diffusion rate equals rate of sublimation critical value, the first controller control heater 11 keeps temperature constant; In the time that diffusion rate is greater than rate of sublimation critical value, the first controller control heater 11 reduces temperature.
In the technique that above-mentioned vacuum sublimation is purified; the keying of taking out in advance valve 4 by second controller control mechanical pump respectively; open by the 3rd controller control molecular pump 9 and molecular pump valve 8; open by the 4th controller control heater 11; and regulate heater 11 by the first controller; realize full-automatic operation, can realize the production of scale.
In this description, each embodiment adopts the mode of going forward one by one to describe, and what each embodiment stressed is and the difference of other embodiment, between each embodiment identical similar part mutually referring to.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (11)
1. the equipment that organic small molecule material vacuum sublimation is purified, comprises quartzy sublimation pipe (1) and the vacuum extractor for described quartzy sublimation pipe (1) is vacuumized; It is characterized in that, also comprise:
The thickness detector (2) of the diffusion rate after the organic small molecule material distillation in described quartzy sublimation pipe (1) can be detected, described thickness detector (2) comprise can with the organic molecule probe (21) that contact after distillation be connected with described probe (21), and send the signal processor (22) of diffusion rate signal;
For the heater (11) that each section of warm area of described quartzy sublimation pipe (1) heated;
Receive described diffusion rate signal, for controlling the regulation device of described heater (11), it regulates control according to received diffusion rate signal to described heater (11), in the time that described diffusion rate is less than the rate of sublimation critical value of setting, make described heater (11) continue the temperature of the described each section of warm area of rising; In the time that described diffusion rate equals described rate of sublimation critical value, make described heater (11) keep the temperature constant of described each section of warm area; In the time that described diffusion rate is greater than described rate of sublimation critical value, make described heater (11) reduce the temperature of described each section of warm area.
2. the equipment that organic small molecule material vacuum sublimation according to claim 1 is purified, it is characterized in that, described regulation device is to be connected with described heater (11), receive the first controller of described diffusion rate signal, described the first controller is made comparisons described diffusion rate and described rate of sublimation critical value, in the time that described diffusion rate is less than described rate of sublimation critical value, control described heater (11) persistently overheating; In the time that described diffusion rate equals described rate of sublimation critical value, control described heater (11) and keep temperature constant; In the time that described diffusion rate is greater than described rate of sublimation critical value, controls described heater (11) and reduce temperature.
3. the equipment that organic small molecule material vacuum sublimation according to claim 2 is purified, is characterized in that, also comprises:
By the manual regulating device of heater (11) described in manual adjustments control; With
The switching device shifter being connected with described manual regulating device with described the first controller respectively.
4. the equipment that organic small molecule material vacuum sublimation according to claim 1 is purified, is characterized in that, described probe (21) is arranged on one end near outlet in described quartzy sublimation pipe (1).
5. the equipment that organic small molecule material vacuum sublimation according to claim 2 is purified, is characterized in that, described vacuum extractor comprises:
Mechanical pump (5), the air entry of described mechanical pump (5) is connected with described quartzy sublimation pipe (1) by the first pipeline (6), and on described the first pipeline (6), is provided with mechanical pump and takes out in advance valve (4);
Molecular pump (9), the air entry of described molecular pump (9) is connected with described quartzy sublimation pipe (1) by the second pipeline (7), exhaust outlet is connected with the air entry of described mechanical pump (5), and is provided with molecular pump valve (8) on described the second pipeline (7).
6. the equipment that organic small molecule material vacuum sublimation according to claim 5 is purified, is characterized in that, also comprises:
Be arranged on described quartzy sublimation pipe (1) upper, for measuring the concurrent vacuum meter (3) that send air pressure signal of air pressure in described quartzy sublimation pipe (1);
Be connected with described vacuum meter (3), receive the second controller of described air pressure signal, in the time that the air pressure in described quartzy sublimation pipe (1) is greater than 50Pa, control described mechanical pump and take out in advance valve (4) unlatching, in the time that described air pressure is less than or equal to 50Pa, controls described mechanical pump and take out in advance valve (4) and close;
Be connected with described vacuum meter (3), receive the 3rd controller of described air pressure signal, in the time that described air pressure is less than or equal to 50Pa, controls described molecular pump (9) and described molecular pump valve (8) simultaneously and open;
Be connected with described vacuum meter (3), receive the 4th controller of described air pressure signal, in the time that described air pressure reaches the vacuum of setting, control described heater and open.
7. the equipment that organic small molecule material vacuum sublimation according to claim 5 is purified, it is characterized in that, the suction opeing of described the first pipeline (6) is connected with described the second pipeline (7) being positioned between described molecular pump valve (8) and described quartzy sublimation pipe (1).
8. the equipment that organic small molecule material vacuum sublimation according to claim 7 is purified, is characterized in that, described the second pipeline (7) is connected by screwed flange with described quartzy sublimation pipe (1), and coordinates by seal with elastometic washer.
9. the equipment of purifying according to the organic small molecule material vacuum sublimation described in claim 1-8 any one, it is characterized in that, the cylindrical quartz pipe of described quartzy sublimation pipe (1) for obtaining by artificial drawing, an end opening of described cylindrical quartz pipe, other end sealing.
10. the technique that organic small molecule material vacuum sublimation is purified, is characterized in that, its equipment that uses the organic small molecule material vacuum sublimation as described in claim 1-9 any one to purify carries out, and comprises step:
1) vacuumize: utilize described vacuum extractor to vacuumize described quartzy sublimation pipe (1), and the air pressure in described quartzy sublimation pipe (1) is measured simultaneously;
2) open described heater (11): in the time that the air pressure in described quartzy sublimation pipe (1) reaches the vacuum of setting, open described heater (11), it is heated each section of warm area of described quartzy sublimation pipe (1);
3) utilize described thickness detector (2) to detect the diffusion rate after the organic small molecule material distillation in described quartzy sublimation pipe (1), and according to described diffusion rate, described heater (11) is regulated, make described diffusion rate finally maintain the rate of sublimation critical value of setting:
In the time that described diffusion rate is less than the rate of sublimation critical value of setting, make described heater (11) continue the temperature of the described each section of warm area of rising; In the time that described diffusion rate equals described rate of sublimation critical value, make described heater (11) keep the temperature constant of described each section of warm area; In the time that described diffusion rate is greater than described rate of sublimation critical value, make described heater (11) reduce the temperature of described each section of warm area.
The technique that 11. organic small molecule material vacuum sublimations according to claim 10 are purified, is characterized in that described step 1) be specially:
11) open the mechanical pump (5) of described vacuum extractor, utilize described in second controller control the mechanical pump of vacuum extractor to take out in advance valve (4) and open, described mechanical pump (5) is vacuumized described quartzy sublimation pipe (1);
12) by vacuum meter (3), the air pressure in described quartzy sublimation pipe (1) is measured, in the time that described air pressure is less than or equal to 50Pa, utilizing described in second controller control mechanical pump to take out in advance valve (4) closes, utilize molecular pump (9) and the molecular pump valve (8) of vacuum extractor described in the 3rd controller control to open simultaneously, described molecular pump (9) and described mechanical pump (5) are linked up described quartzy sublimation pipe (1) is vacuumized;
Described step 2) be specially:
Open by heater (11) described in the 4th controller control, described heater (11) is resistive heating device;
Described step 3) specifically by the first controller, described heater (11) is regulated, in the time that described diffusion rate is less than described rate of sublimation critical value, heater (11) is persistently overheating described in described the first controller control; In the time that described diffusion rate equals described rate of sublimation critical value, heater (11) keeps temperature constant described in described the first controller control; In the time that described diffusion rate is greater than described rate of sublimation critical value, heater (11) reduces temperature described in described the first controller control.
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| CN107376394A (en) * | 2017-08-04 | 2017-11-24 | 贵州自然生物科技有限公司 | Sublimed method pyrogallic acid automatically adjusts speed of exhaust retracting device |
| CN108854136B (en) * | 2018-07-20 | 2021-02-26 | 合肥欧莱迪光电技术有限公司 | Special equipment for purifying visible organic small molecules in high vacuum in open mode |
| CN108854118A (en) * | 2018-08-02 | 2018-11-23 | 苏州大学 | A kind of low dose organic material method of purification and equipment for purifying |
| CN109646987B (en) * | 2019-01-10 | 2024-03-26 | 合肥百思智能装备有限公司 | Continuous feeding and discharging high-vacuum organic micromolecule purifying special equipment |
| CN113694559B (en) * | 2021-08-30 | 2022-09-27 | 四川阿格瑞新材料有限公司 | Organic material purification system and use method |
| CN114558343B (en) * | 2022-02-28 | 2023-05-05 | 中国科学院长春应用化学研究所 | Vacuum sublimation purification device |
| CN114405046B (en) * | 2022-02-28 | 2023-08-29 | 中国科学院长春应用化学研究所 | Cooling device based on vacuum sublimation purification equipment |
| CN114534298A (en) * | 2022-02-28 | 2022-05-27 | 中国科学院长春应用化学研究所 | Purification method, system and device |
| CN114534299B (en) * | 2022-02-28 | 2022-10-28 | 中国科学院长春应用化学研究所 | Diffusion rate adjusting method, system, device and storage medium |
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| CN2710718Y (en) * | 2004-08-03 | 2005-07-20 | 山西至诚科技有限公司 | Vacuum sublimation appts suitable for collecting products |
| CN100998928A (en) * | 2006-01-13 | 2007-07-18 | 中国科学院半导体研究所 | Sublimation purification device of organic material |
| CN201664523U (en) * | 2010-03-26 | 2010-12-08 | 陕西科技大学 | Sublimation purification device of organic materials |
| CN102527076B (en) * | 2010-12-31 | 2014-04-30 | 上海广茂达光艺科技股份有限公司 | Vacuum sublimation purifying method of OLED (organic light emitting diode) material |
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