阅读说明：本技术 一种量产型自动保护有机小分子提纯设备的升华仪 (Mass production type sublimation instrument for automatically protecting organic small molecule purification equipment ) 是由 孔令杰 李晓丽 于 2020-06-10 设计创作，主要内容包括：本发明公开了一种量产型自动保护有机小分子提纯设备的升华仪,设置的阻挡机构,利用阻挡机构中的旋转挡板、传动轴、磁流体、联轴器和气缸的配合使用,可以将提纯材料加热过程中的杂质气体进行隔离收集,避免杂质气体进入至分子泵中,对分子泵的运行和真空座内的真空度造成影响,克服了现有方案中不能对杂质气体进行处理,导致杂质气体进入至分子泵中,对分子泵的工作造成影响,进而影响真空座内的真空度以及提纯材料的加工效果；设置的双层冷井和阻挡机构的配合使用,部分杂质气体穿过旋转挡板后进入双层冷井,通过双层冷井对杂质气体进行降温冷却,可以进一步提高对杂质气体的处理效果,克服了杂质气体处理的效率不佳的缺陷。(The invention discloses a sublimation instrument for mass production type automatic protection of organic small molecule purification equipment, which is provided with a blocking mechanism, wherein the blocking mechanism is used for isolating and collecting impurity gas in the heating process of a purification material by utilizing the matching use of a rotary baffle, a transmission shaft, a magnetic fluid, a coupler and a cylinder in the blocking mechanism, so that the influence on the operation of a molecular pump and the vacuum degree in a vacuum seat caused by the impurity gas entering the molecular pump is avoided, and the defects that the impurity gas cannot be treated in the existing scheme, the impurity gas enters the molecular pump, the operation of the molecular pump is influenced, and the vacuum degree in the vacuum seat and the processing effect of the purification material are further influenced are overcome; the double-deck cold well that sets up and stop gear's cooperation are used, and partial impurity gas gets into double-deck cold well after passing rotating barrier, cools down the cooling to impurity gas through double-deck cold well, can further improve the treatment effect to impurity gas, has overcome the not good defect of efficiency that impurity gas handled.)

1. The utility model provides a sublimator of automatic protection organic small molecule purification equipment of volume production type, a serial communication port, including stop gear (101) and heating seat (3), stop gear (101) are located one side of heating seat (3), stop gear (101) contain rotating barrier (6), transmission shaft (7), magnetic fluid (8), shaft coupling (9) and cylinder (10), rotating barrier (6) are located the top, cylinder (10) are located the bottom, transmission shaft (7), magnetic fluid (8) and shaft coupling (9) are located the position between rotating barrier (6) and cylinder (10), magnetic fluid (8) are located the position between transmission shaft (7) and shaft coupling (9), transmission shaft (7) are located the top of shaft coupling (9), workstation (1) is installed to the below of stop gear (101), one side of the rotary baffle plate (6) is connected with a vacuum seat (2), an observation window (13) is installed on the outer surface of the vacuum seat (2), an adjustable box body (16) is arranged on one side of the workbench (1), a guide pipe is connected to the upper end of the adjustable box body (16), a gate valve (11), a double-layer cold well (12) and an ionization gauge (14) are installed above the adjustable box body (16), the double-layer cold well (12) is located between the gate valve (11) and the ionization gauge (14), the gate valve (11) is located on one side of the ionization gauge (14), the rotary baffle plate (6) is located inside the guide pipe and close to one side of the guide pipe, and one side, far away from the double-layer cold well (12), of the ionization gauge (14) is connected with a molecular pump (15);

supporting seat (20) are installed to the lower extreme of heating seat (3), detect flange (17) are installed to one side of heating seat (3), special flange (19) are installed to the opposite side of heating seat (3), a plurality of test tube (18) are installed to the surface of heating seat (3) near the position that detects flange (17).

2. The sublimation meter of mass production type automatic protection organic small molecule purification equipment according to claim 1, characterized in that, the operation screen is installed to the front end of workstation (1), the lower extreme of push-pull valve (11) runs through to the inside of pipe, workstation (1) is located the position between heating seat (3) and special flange (19), fixedly connected with connecting pipe between heating seat (3) and vacuum seat (2), the upper end of vacuum seat (2) is connected with resistance gauge (4), install other valve (5) of taking out between resistance gauge (4) and push-pull valve (11), other valve (5) of taking out is located the top of rotating barrier (6).

3. The sublimation apparatus for mass production type automatic protection of small organic molecule purification equipment according to claim 1, wherein the installation manner of the rotating baffle (6) is a shutter form, a plurality of baffle bodies and a fixing ring are arranged inside the rotating baffle (6), and the plurality of fixing rings are located inside the baffle bodies near the middle position.

4. The sublimation apparatus for mass production type automatic protection of organic small molecule purification equipment according to claim 3, wherein the transmission shaft (7) is fixedly connected with the plurality of baffle bodies through a fixing ring, and the upper end of the transmission shaft (7) is fixedly connected with the inner surface of the rotating baffle (6) at a position close to the upper end.

5. The sublimator of the mass production type automatic protection organic small molecule purifying equipment according to claim 1, wherein the lower end of the coupling (9) penetrates into the cylinder (10), and the magnetic fluid (8) is connected with the cylinder (10) in a sliding manner through the coupling (9).

6. The sublimation apparatus for the mass production type automatic protection of the organic small molecule purification equipment according to claim 1, wherein the rotating baffle (6) rotates up and down in the vertical direction through the transmission shaft (7) and the magnetic fluid (8), and the angle range of the up and down rotation of the rotating baffle (6) is-90 ° to 90 °.

7. The sublimation apparatus for the mass production type automatic protection of the small organic molecule purification equipment according to claim 1, wherein the molecular pump (15) is fixedly connected with the vacuum base (2) through a conduit, the vacuum base (2) is made of quartz glass, a vacuum chamber is arranged inside the vacuum base (2), and a plurality of heating furnaces are arranged inside the heating base (3).

8. The sublimation apparatus for the mass production type automatic protection of the small organic molecule purification equipment according to any one of claims 1 to 7, wherein the operation steps of the sublimation apparatus for the mass production type automatic protection of the small organic molecule purification equipment are as follows:

the method comprises the following steps: opening a detection flange (17), loading materials to be purified in a test tube (18), detecting the internal temperature of the test tube (18) through the detection flange (17), adjusting the temperature difference between the inside and the outside of the test tube (18), lifting a coupler (9) through an air cylinder (10), and transmitting a transmission shaft (7) and a magnetic fluid (8) through the lifting transmission of the coupler (9) to enable a rotary baffle (6) to be in an opening and closing state, starting a molecular pump (15), and carrying out vacuum treatment on a vacuum seat (2) through a conduit;

step two: the coupler (9) is descended through the air cylinder (10), the transmission shaft (7) and the magnetic fluid (8) are descended through the coupler (9) to enable the rotary baffle (6) to be in a closed state, the heating seat (3) is utilized to heat and react and purify the purification material in the test tube (18), and impurities generated in the heating process of the purification material are isolated by the closed rotary baffle (6);

step three: part of the impurity gas passes through the rotary baffle (6) and then enters the double-layer cold well (12), and the impurity gas is cooled through the double-layer cold well (12), so that the impurity gas is cooled and deposited in the double-layer cold well (12);

step four: after the impurity gas is treated, the coupler (9) is lifted through the air cylinder (10), the transmission shaft (7) and the magnetic fluid (8) are transmitted through the lifting of the coupler (9), the rotating baffle (6) is in an opening and closing state, the vacuum degree in the vacuum seat is detected through the resistance gauge (4), the process operation is carried out on the purified material, after the process operation is finished, the special flange (19) is opened, and the treated purified material is collected.

Technical Field

The invention relates to the technical field of organic small molecule purification, in particular to a mass production type sublimation instrument for automatically protecting organic small molecule purification equipment.

Background

The sublimation instrument is mainly used for sublimating an organic mixture under a vacuum condition to achieve the purpose of purification, and the main processed object is an organic material with sublimation property or a mixture with mobile phase characteristics such as an organic acousto-optic product or a nano material.

According to the existing mass production type purification equipment, because the purification of organic small molecular materials needs to be carried out under the vacuum condition provided by a molecular pump, the required materials are separated from impurities, however, certain impurities can be naturally decomposed under the vacuum condition in the process, and the impurities enter the molecular pump along with gas under the action of gas flow, so that the molecular pump is polluted, and the equipment cannot normally operate.

Disclosure of Invention

The invention aims to provide a mass production type sublimation instrument for automatically protecting organic small molecule purification equipment, and solves the technical problems that: how to prevent the impurity substance from flowing along with the gas to pollute the molecular pump, and simultaneously ensure that the pumping speed of the molecular pump is not influenced, and avoid the failure of the material due to cracking.

The purpose of the invention can be realized by the following technical scheme:

the utility model provides a volume production type automatic protection organic small molecule purification equipment's sublimometer, includes stop mechanism and heating seat, stop mechanism is located one side of heating seat, stop mechanism contains rotating barrier, transmission shaft, magnetic fluid, shaft coupling and cylinder, rotating barrier is located the top, the cylinder is located the lower extreme, transmission shaft, magnetic fluid and shaft coupling are located the position between rotating barrier and the cylinder, the magnetic fluid is located the position between transmission shaft and the shaft coupling, the transmission shaft is located the top of shaft coupling, the workstation is installed to stop mechanism's below, one side of rotating barrier is connected with the vacuum seat, the surface mounting of vacuum seat has the observation window, one side of workstation is provided with adjustable box, the upper end of adjustable box is connected with the pipe, push-pull valve, vacuum seat are installed to the top of adjustable box, The double-layer cold well is positioned between a gate valve and an ionization gauge, the gate valve is positioned on one side of the ionization gauge, the rotating baffle is positioned in the position close to one side in the guide pipe, and one side, far away from the double-layer cold well, of the ionization gauge is connected with a molecular pump;

the supporting seat is installed to the lower extreme of heating seat, the detection flange is installed to one side of heating seat, special flange is installed to the opposite side of heating seat, a plurality of test tube is installed to the surface of heating seat near the position that detects the flange.

Further, the operation screen is installed to the front end of workstation, the lower extreme of push-pull valve runs through to the inside of pipe, the workstation is located the position between heating seat and the special flange, fixedly connected with connecting pipe between heating seat and the vacuum seat, the upper end of vacuum seat is connected with the resistance rule, install other pump valve between resistance rule and the push-pull valve, other pump valve is located rotating baffle's top.

Further, the mounting means of whirl baffle is the shutter form, whirl baffle's inside is provided with a plurality of baffle body and solid fixed ring, and the inside that a plurality of solid fixed ring is located the baffle body is close to the position in the middle.

Further, the transmission shaft is fixedly connected with the plurality of baffle bodies through a fixing ring, and the upper end of the transmission shaft is fixedly connected with the inner surface of the rotating baffle close to the upper end.

Further, the lower end of the coupler penetrates into the cylinder, and the magnetic fluid is connected with the cylinder in a sliding mode through the coupler.

Further, the rotary baffle plate rotates up and down in the vertical direction through the transmission shaft and the magnetic fluid, and the angle range of the up-and-down rotation of the rotary baffle plate is-90 degrees to 90 degrees.

Furthermore, the molecular pump is fixedly connected with a vacuum seat through a conduit, the vacuum seat is made of quartz glass, a vacuum cavity is arranged in the vacuum seat, and a plurality of heating furnaces are arranged in the heating seat.

Further, the operation steps of the sublimation apparatus for the mass production type automatic protection organic small molecule purification equipment are as follows:

the method comprises the following steps: opening a detection flange, loading a material to be purified in a test tube, detecting the internal temperature of the test tube through the detection flange, adjusting the temperature difference between the inside and the outside of the test tube, lifting a coupler through a cylinder, and driving a transmission shaft and a magnetic fluid through the lifting transmission of the coupler to enable a rotary baffle to be in an open-close state, starting a molecular pump, and performing vacuum treatment on a vacuum seat through a guide pipe;

step two: the coupler is descended through the air cylinder, the transmission shaft and the magnetic fluid are driven through descending of the coupler, so that the rotary baffle is in a closed state, the purifying material in the test tube is heated and reacted and purified by the heating seat, and impurities generated in the heating process of the purifying material are isolated by the closed rotary baffle;

step three: part of the impurity gas passes through the rotary baffle plate and then enters the double-layer cold well, and the impurity gas is cooled through the double-layer cold well, so that the impurity gas is cooled and deposited in the double-layer cold well;

step four: after the impurity gas is treated, the coupler is lifted through the air cylinder, the transmission shaft and the magnetic fluid are transmitted through the lifting of the coupler, the rotary baffle is in an opening and closing state, the vacuum degree in the vacuum seat is detected through the resistance gauge, the process operation is carried out on the purification material, after the process operation is finished, the special flange is opened, and the treated purification material is collected.

The invention has the beneficial effects that:

(1) the invention can isolate and collect the impurity gas in the heating process of the purifying material by the matched use of the rotary baffle plate, the transmission shaft, the magnetic fluid, the coupling and the air cylinder in the blocking mechanism through the arranged blocking mechanism, so as to avoid the impurity gas from entering the molecular pump to influence the running of the molecular pump and the vacuum degree in the vacuum seat, the coupling is lifted through the air cylinder, the transmission shaft and the magnetic fluid are driven by the lifting of the coupling to ensure that the rotary baffle plate is in an open-close state, the molecular pump is started, the vacuum seat is subjected to vacuum treatment through the conduit, the coupling is lowered through the air cylinder, the transmission shaft and the magnetic fluid are driven by the lowering of the coupling to ensure that the rotary baffle plate is in a close state, the purifying material in the test tube is heated and reacted and purified by the heating seat, and the impurities generated in the heating process of the purifying, the processing efficiency of the purified material can be effectively improved, and the defect that the impurity gas cannot be processed in the existing scheme, so that the impurity gas enters the molecular pump to influence the work of the molecular pump, and further influence the vacuum degree in the vacuum seat and the processing effect of the purified material is overcome;

(2) according to the invention, the double-layer cold well and the blocking mechanism are matched for use, so that the treatment effect on the impurity gas can be effectively improved, the impurity gas is isolated and blocked by the blocking mechanism, part of the impurity gas passes through the rotary baffle plate and then enters the double-layer cold well, and the impurity gas is cooled and deposited in the double-layer cold well through the double-layer cold well, so that the treatment effect on the impurity gas can be further improved, and the defect of poor impurity gas treatment efficiency caused by poor sealing property of impurity gas isolation is overcome.

Drawings

In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.

FIG. 1 is a schematic view of a connection structure of a sublimation apparatus for mass production type automatic protection of organic small molecule purification equipment;

FIG. 2 is a schematic side view of the connection structure of the workbench according to the present invention.

In the figure: 1. a work table; 101. a blocking mechanism; 2. a vacuum seat; 3. a heating base; 4. a resistance gauge; 5. a side pumping valve; 6. rotating the baffle; 7. a drive shaft; 8. a magnetic fluid; 9. a coupling; 10. a cylinder; 11. a gate valve; 12. a double-layer cold well; 13. an observation window; 14. an ionization gauge; 15. a molecular pump; 16. an adjustable box body; 17. detecting the flange; 18. a test tube; 19. a special flange; 20. and (4) supporting the base.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

As shown in fig. 1-2, a mass production type sublimation apparatus for automatically protecting organic small molecule purification equipment comprises a blocking mechanism 101 and a heating base 3, wherein the blocking mechanism 101 is located on one side of the heating base 3, the blocking mechanism 101 comprises a rotary baffle 6, a transmission shaft 7, a magnetic fluid 8, a coupling 9 and a cylinder 10, the rotary baffle 6 is located at the uppermost end, the cylinder 10 is located at the lowermost end, the transmission shaft 7, the magnetic fluid 8 and the coupling 9 are located at positions between the rotary baffle 6 and the cylinder 10, the magnetic fluid 8 is located at positions between the transmission shaft 7 and the coupling 9, the transmission shaft 7 is located above the coupling 9, a worktable 1 is installed below the blocking mechanism 101, one side of the rotary baffle 6 is connected with a vacuum base 2, an observation window 13 is installed on the outer surface of the base 2, one side of the worktable 1 is provided with an adjustable box 16, the upper end of the adjustable box body 16 is connected with a guide pipe, a gate valve 11, a double-layer cold well 12 and an ionization gauge 14 are mounted above the adjustable box body 16, the double-layer cold well 12 is located between the gate valve 11 and the ionization gauge 14, the gate valve 11 is located on one side of the ionization gauge 14, the rotating baffle 6 is located inside the guide pipe and close to one side, and one side, far away from the double-layer cold well 12, of the ionization gauge 14 is connected with a molecular pump 15;

supporting seat 20 is installed to the lower extreme of heating seat 3, detection flange 17 is installed to one side of heating seat 3, special flange 19 is installed to the opposite side of heating seat 3, a plurality of test tube 18 is installed to the surface of heating seat 3 near the position that detects flange 17.

The operation screen is installed to the front end of workstation 1, the lower extreme of push-pull valve 11 runs through to the inside of pipe, workstation 1 is located the position between heating seat 3 and the special flange 19, fixedly connected with connecting pipe between heating seat 3 and the vacuum seat 2, the upper end of vacuum seat 2 is connected with resistance gauge 4, install other valve 5 of taking out between resistance gauge 4 and the push-pull valve 11, other valve 5 of taking out is located the top of rotating barrier 6.

The mounting means of whirl baffle 6 is the shutter form, whirl baffle 6's inside is provided with a plurality of baffle body and solid fixed ring, and the inside that a plurality of solid fixed ring is located the baffle body is close to the position in the middle.

The transmission shaft 7 is fixedly connected with the plurality of baffle bodies through a fixing ring, and the upper end of the transmission shaft 7 is fixedly connected with the inner surface of the rotating baffle 6 close to the upper end.

The lower end of the coupler 9 penetrates into the cylinder 10, and the magnetic fluid 8 is connected with the cylinder 10 in a sliding mode through the coupler 9.

The rotating baffle 6 rotates up and down in the vertical direction through the transmission shaft 7 and the magnetic fluid 8, and the angle range of the up-and-down rotation of the rotating baffle 6 is-90 degrees.

The molecular pump 15 is fixedly connected with the vacuum seat 2 through a conduit, the vacuum seat 2 is made of quartz glass, a vacuum cavity is arranged in the vacuum seat 2, and a plurality of heating furnaces are arranged in the heating seat 3.

The operation steps of the sublimation instrument for the mass production type automatic protection organic small molecule purification equipment are as follows:

the method comprises the following steps: opening the detection flange 17, loading a material to be purified in the test tube 18, detecting the internal temperature of the test tube 18 through the detection flange 17, adjusting the temperature difference between the inside and the outside of the test tube 18, lifting the coupling 9 through the air cylinder 10, and driving the transmission shaft 7 and the magnetic fluid 8 through the lifting transmission of the coupling 9 to enable the rotating baffle 6 to be in an opening and closing state, starting the molecular pump 15, and performing vacuum treatment on the vacuum seat 2 through a conduit;

step two: the coupler 9 is descended through the air cylinder 10, the transmission shaft 7 and the magnetic fluid 8 are descended through the coupler 9 to enable the rotary baffle 6 to be in a closed state, the heating seat 3 is utilized to heat and react and purify the purification material in the test tube 18, and impurities generated in the heating process of the purification material are isolated by the closed rotary baffle 6;

step three: part of the impurity gas passes through the rotary baffle 6 and then enters the double-layer cold well 12, and the impurity gas is cooled through the double-layer cold well 12, so that the impurity gas is cooled and deposited in the double-layer cold well 12;

step four: after the impurity gas is treated, the coupling 9 is lifted through the air cylinder 10, the transmission shaft 7 and the magnetic fluid 8 are transmitted through the lifting of the coupling 9, the rotating baffle 6 is in an opening and closing state, the vacuum degree in the vacuum seat is detected through the resistance gauge 4, the process operation is carried out on the purified material, after the process operation is finished, the special flange 19 is opened, and the treated purified material is collected.

Various aspects disclosed in the embodiments of the present invention: through the arranged blocking mechanism 101, the impurity gas in the heating process of the purification material can be isolated and collected by utilizing the matching use of the rotary baffle 6, the transmission shaft 7, the magnetic fluid 8, the coupler 9 and the air cylinder 10 in the blocking mechanism 101, the impurity gas is prevented from entering the molecular pump 15 and influencing the operation of the molecular pump 15 and the vacuum degree in the vacuum seat 2, the coupler 9 is lifted through the air cylinder 10, the transmission shaft 7 and the magnetic fluid 8 are driven by the lifting of the coupler 9, so that the rotary baffle 6 is in an opening and closing state, the molecular pump 15 is started, the model of the molecular pump 15 can be 2XZ type, the vacuum seat 2 is subjected to vacuum treatment through a conduit, the coupler 9 is lowered through the air cylinder 10, the transmission shaft 7 and the magnetic fluid 8 are driven by the descending of the coupler 9, so that the rotary baffle 6 is in a closing state, the purification material in the test tube 18 is heated and reacted and purified by utilizing the heating, impurities generated in the heating process of the purification material are isolated by the closed rotary baffle 6, so that the processing efficiency of the purification material can be effectively improved, and the defects that the impurity gas cannot be treated in the existing scheme, the impurity gas enters the molecular pump 15, the operation of the molecular pump 15 is influenced, and the vacuum degree in the vacuum seat 2 and the processing effect of the purification material are further influenced are overcome;

the cooperation through the double-deck cold well 12 that sets up and blocking mechanism 101 is used, can effectively improve the treatment effect to gaseous impurity, gaseous impurity is through the isolation of blocking mechanism 101 with block the back, partial gaseous impurity enters double-deck cold well 12 after passing rotating barriers 6, cool down the cooling to gaseous impurity through double-deck cold well 12, make gaseous impurity cooling and deposit in double-deck cold well 12, and then can further improve the treatment effect to gaseous impurity, overcome the poor not good defect of efficiency that leads to gaseous impurity to handle of the leakproofness difference that gaseous impurity kept apart.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.