CN1535749A

CN1535749A - Improved sublimation purification method

Info

Publication number: CN1535749A
Application number: CNA031095941A
Authority: CN
Inventors: 张书文; 林国森; 陈奇民
Original assignee: SHENGYUAN SCI-TECH Co Ltd
Current assignee: Wintek Corp
Priority date: 2003-04-11
Filing date: 2003-04-11
Publication date: 2004-10-13

Abstract

The present invention relates to an improved sublimation purification method. It utilizes a preset pressure, temp. and time to compress the powdered material to be purified into compact granules or ingot-like material firstly, because the compressed material to be purified is compacter than powdered material, so that unit volume can receive still more material to be purified, and can make the heat transfer efficiency of compressed material to be purified be raised, make the heating power be more stable, and in the sublimatiojn purification process a flowable inert gas can be added, and the inert gas can be used for carrying the sublimed purified material to make the purified material be flowed toward same direction and be deposited.

Description

Improved sublimation purification method

Technical field

The present invention relates to a kind of improved sublimation purification method, the improvement of the making flow and method when particularly pulverous thing to be purified uses sublimation purification.

Background technology

Sublimation purification mainly is by heat energy, impel mixture to be transformed into the operation of two-phase, comprise that gaseous state separates with liquid state, and gaseous state and the solid-state integration utilization that technology such as separates, close or have a mixture systems that common boiling point is formed at boiling point, also can reach the purpose of refining purifying by the introducing of technology such as common boiling point distillation distillation or extractive distillation distillation.

The sublimation purification mode all is filled to sublimator with pulverous thing to be purified at present, heating sublimation thing to be purified reaches the purpose of sublimation purification under vacuum environment, but thing to be purified is but because be Powdered, it organizes looser, and between each thing to be purified the space is arranged, because this space causes heat-conducting effect not good, especially under the vacuum state when sublimation purification, the not good situation of heat-conducting effect is more obvious.

So organize looser because thing to be purified is Powdered its, thereby the quality in its unit volume is limited, cause once the collecting amount of thing sublimation purification to be purified few, if reach predetermined required purifying thing amount, just essential sublimation purification repeatedly, if need to replace thing to be purified and just must open the door of purifying chamber and run into during sublimation purification, and the door that will open a purifying chamber just must be done the action of once lowering the temperature and bleeding, and must once bleed and heat after having changed thing to be purified, this motion flow is not only lost time, and has also increased the bad probability of purifying.

And general sublimation purification mode makes purifying logistics after the distillation to any direction, and the purifying thing deposition on each collection unit is disperseed, and causes the time waste in the collection.

Summary of the invention

Main purpose of the present invention, be to address the aforementioned drawbacks, for avoiding the existence of this defective, utilization of the present invention is by a predetermined pressure, predetermined temperature and required time, earlier pulverous thing to be purified is pressed into compact shape, finish thing to be purified after the compacting when sublimation purification, because the thing to be purified after the compacting is more Powdered more fine and close, unit volume can be held the more thing to be purified of multimass, make the collected purifying substance amount of flow process so can increase the single sublimation purification, all helpful to the probability that the saving on the activity duration is bad with reducing purifying.

And because the thing even compact to be purified after the compacting, there is not the space between each thing to be purified, because this space causes the not good situation of heat-conducting effect also not exist, use the thing to be purified of compacting back compact shape that the heat conduction efficiency between each thing to be purified is improved, because the raising of heat conduction efficiency makes heat transfer rate faster, saved the energy that is used to heat, being used the inert gas that flows to be aided with the purifying thing deposits at a fixed-direction, and replace original air with inert gas, pressure in the time of can making sublimation purification is 0.1torr, do not need under high vacuum state, to do sublimation purification, manufacture the time of flow process for purifying and save, the pressure control during with sublimation purification will be more easy.

Description of drawings

Fig. 1 is the manufacturing process schematic diagram of improved sublimation purification method of the present invention.

Fig. 2 is the purifying schematic diagram of improved sublimation purification method of the present invention.

The specific embodiment

Relevant detailed description of the present invention and technology contents, existing as follows with regard to accompanying drawings:

See also shown in Figure 1, it is the manufacturing process schematic diagram of the improved sublimation purification method of the present invention, as shown in the figure: be by a predetermined pressure, temperature and time, earlier pulverous thing 10 to be purified is pressed into compact shape, finish thing to be purified 10 after the compacting when sublimation purification, because the thing to be purified 10 more Powdered more even compacts after the compacting, so unit volume can be held the more thing to be purified 10 of multimass, the carrier 211 of i.e. distillation portion 21 thing to be purified 10 quality that are loaded with that once distil increase greatly, and because thing to be purified 10 even compacts after the compacting, thing to be purified 10 unlike the starting powder shape, there has not been the space between each thing 10 to be purified, heat conduction efficiency is improved, heating power is more stable, and when collecting the purifying thing 11 of distillation, utilizes the inert gas that flows as carrying gas, it is more concentrated that purifying thing 11 is collected, and the sublimation purification step behind this sublimation purification method improvement includes:

A) getting is pulverous thing to be purified 10 originally, by predetermined pressure, temperature and time pulverous thing 10 to be purified is pressed into compact shape, wherein, this predetermined pressure is that 5000 (pound/square inches) to 50000 (pound/square inches), temperature is that 20 degree Celsius to 120 degree, the time is 20 minutes to 60 minutes, adjust according to the form crystal lattice of required thing to be purified 10 and compactness extent and the character that do not influence thing 10 to be purified, this compact shape sample attitude can be graininess or ingot shape;

B) see also shown in Figure 2, it is the purifying schematic diagram of sublimation purification method improvement of the present invention, as shown in the figure: will be seated in the distillation portion 21 of purification devices 20 1 ends through the thing to be purified 10 after the compacting of step a making flow process, this distillation portion 21 is provided with a carrier 211 devices thing to be purified 10 to be distilled, and this purification devices 20 is connected the collection unit more than two 22 that distillation portion 21 is provided with;

C) utilize a steam vent 23 that is connected vacuum system 30 that is arranged on purification devices 20 other ends, this vacuum system 30 makes the state that forms 0.1torr (atmospheric pressure is 760torr) in the purification devices 20 by steam vent 23 pumped down;

D) utilize an inert gas installation 40 to be connected the air admission hole 24 that purification devices 20 is arranged on distillation portion 21 ends, inert gas is entered in the purification devices 20 according to set rate, and vacuum system 30 is bled by steam vent 23 according to set rate, inert gas stopped to enter when this vacuum system 30 was bled, and inert gas when entering vacuum system 30 stop to bleed, so for several times make the air that does not exhaust of the former purification devices 20 of inert gas replacement, and form the states of 0.1torr (atmospheric pressure is 760torr) this moment in the inert gas purification devices 20;

E) utilize one to be located at purification devices 20 outsides and to impel thing 10 distillations to be purified with respect to a heater 50 heating of the position of distillation portion 21, this distillation portion 21 is subjected to the temperature of heater 50 heating between 200 degree Celsius are spent to 500, heating-up temperature is controlled according to the character of thing 10 to be purified, and when heater 50 heating impel thing 10 distillations to be purified, this inert gas enters purification devices 20 by air admission hole 24 according to predetermined speed, inert gas is discharged by steam vent 23 simultaneously, making inert gas keep a set rate in purification devices 20 flows, the purifying thing 11 of distillation is flowed to collection unit 22 with inert gas, the purifying thing 11 of distillation this moment is low than distillation portion 21 because of temperature in collection unit 22 inner meetings, and makes purifying thing 11 be deposited on the inwall of collection unit 22;

F) after purifying was made the flow process end, by taking out collection units 22 in the purification devices 20, the inwall of collection unit 22 was made in the flow process at purifying and is deposited purifying thing 11 at this moment, collects this purifying thing 11.

In addition, the thing to be purified 10 in the above-mentioned steps is that an organic or inorganic material is made, and this inert gas is nitrogen, argon gas or helium.

Above-mentioned is preferred embodiment of the present invention only, is not to be used for limiting scope of the invention process.Be that all equalizations of being done according to the present patent application claim change and modification, be all claim of the present invention and contain.

Claims

1. improved sublimation purification method, be earlier pulverous thing to be purified (10) to be pressed into compact shape, because the thing described to be purified (10) after the compacting is more Powdered more fine and close, unit volume can be held the more thing described to be purified (10) of multimass, and because thing described to be purified (10) even compact after the compacting, the heat conduction efficiency of described thing to be purified (10) is improved, it is characterized in that the step of the sublimation purification behind the described sublimation purification method improvement includes:

A) by predetermined pressure, temperature and time pulverous described thing to be purified (10) is pressed into compact shape;

B) will insert purification devices (20) through the thing described to be purified (10) that described step a makes after flow process is suppressed, described thing to be purified (10) places the carrier (211) of distillation portion (21);

C) utilize an inert gas installation described inert gas to be entered in the described purification devices (20), and bleed, make the original air of described inert gas replacement by steam vent (23) by air admission hole (24);

D) utilize a vacuum system by described steam vent (23) pumped down, make the state that forms 0.1torr in the described purification devices (20);

E) utilize a heater (a 50) heating of being located at the outside position with respect to described distillation portion (21) of described purification devices (20) to impel described thing to be purified (10) to reach sublimation condition;

F) the purifying thing on the collection collection unit (22).

2. a kind of improved sublimation purification method according to claim 1 is characterized in that described thing to be purified (10) is that an organic or inorganic material is made.

3. a kind of improved sublimation purification method according to claim 1, it is characterized in that, described predetermined pressure be 5000 (pound/square inches) to 50000 (pound/square inches), adjust according to the compactness extent of required thing described to be purified (10) and the character that do not influence described thing to be purified.

4. a kind of improved sublimation purification method according to claim 1, it is characterized in that, described predetermined temperature be 20 degree Celsius to 120 degree, adjust according to the compactness extent of required thing described to be purified (10) and the character that do not influence described thing to be purified (10).

5. a kind of improved sublimation purification method according to claim 1, it is characterized in that, the described scheduled time is 20 minutes to 60 minutes, adjusts according to the compactness extent of required thing described to be purified (10) and the character that do not influence described thing to be purified (10).

6. a kind of improved sublimation purification method according to claim 1 is characterized in that described compact shape sample attitude can be graininess or ingot shape.

7. a kind of improved sublimation purification method according to claim 1, it is characterized in that, described steam vent (23) is positioned at the other end that described purification devices (20) is put described distillation portion (21), and described air admission hole (24) is arranged at and the corresponding end of described steam vent (23).

8. a kind of improved sublimation purification method according to claim 1 is characterized in that described inert gas is nitrogen, argon gas, helium.

9. a kind of improved sublimation purification method according to claim 1 is characterized in that, it is that 200 degree Celsius are to 500 degree that described distillation portion (21) is subjected to the temperature of described heater (50) heating.

10. a kind of improved sublimation purification method according to claim 1, it is characterized in that, described thing to be purified (10) is when reaching sublimation condition, described inert gas enters described purification devices (20) by described air admission hole (24) according to desired rate, discharges described inert gas by described steam vent (23) simultaneously.