CN114798125A - Vacuum freezing grinding device and method - Google Patents
Vacuum freezing grinding device and method Download PDFInfo
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- CN114798125A CN114798125A CN202210404754.8A CN202210404754A CN114798125A CN 114798125 A CN114798125 A CN 114798125A CN 202210404754 A CN202210404754 A CN 202210404754A CN 114798125 A CN114798125 A CN 114798125A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
- B02C19/186—Use of cold or heat for disintegrating
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L19/00—Details of, or accessories for, apparatus for measuring steady or quasi-steady pressure of a fluent medium insofar as such details or accessories are not special to particular types of pressure gauges
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Abstract
The invention provides a vacuum freezing and grinding device and a method. The freezing chamber is arranged in the vacuum chamber; the main machine of the refrigerating device is positioned outside the vacuum chamber; the reciprocating device is installed in the vacuum chamber, and an upper reciprocating shaft and a lower reciprocating shaft of the reciprocating device penetrate through the bottom of the freezing chamber to the inside of the freezing chamber. During the use, the sample of freezing cavity is frozen through refrigerating plant earlier, and rethread vacuum generator draws the vacuum in to vacuum chamber and the freezing cavity, and reciprocating motion device drives sample tube high frequency reciprocating motion at last, accomplishes the sample and grinds. Freezing and grinding are all accomplished at freezing cavity, reduce cold volume loss, grind after the evacuation again, do not have the hindrance of air during high frequency reciprocating motion, reduced the noise, sample cold volume loss is little, ensures that the sample characteristic is stable around grinding, promotes grinding efficiency, can obtain the sample of lower fineness.
Description
Technical Field
The invention relates to the technical field of crushing and grinding, in particular to a vacuum freezing and grinding device and method.
Background
The advantages of low-temperature freeze grinding are obvious, the low-temperature grinding sample can effectively inhibit degradation, and the activity of the sample is retained; for high-toughness, high-strength and difficult-to-grind samples, the grinding effect and efficiency can be greatly improved by freeze grinding. However, in the existing low-temperature freezing grinding technology, the grinding is carried out under normal pressure, the high-frequency reciprocating motion can aggravate airflow flow during grinding, the loss of cold energy is fast, the local temperature rise is fast, and the temperature of a sample is difficult to stably keep in a low-temperature state.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention aims to provide a vacuum freeze grinding device and a method.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: a vacuum freeze grinding apparatus comprising:
the vacuum chamber is provided with a first vacuumizing interface on a wall body;
the freezing chamber is arranged in the vacuum chamber, a discharge hole is formed above the freezing chamber, and a sealing cover capable of being opened and closed is arranged at the discharge hole;
a vacuum generating device for drawing a vacuum to the vacuum chamber and the freezing chamber;
the refrigerating device is used for providing a cold source for the freezing chamber, and a main machine of the refrigerating device is positioned outside the vacuum chamber;
the reciprocating device is arranged in the vacuum chamber, and an upper reciprocating shaft and a lower reciprocating shaft of the reciprocating device penetrate through the freezing chamber from the bottom of the freezing chamber;
the adapter is used for placing a sample tube and is arranged at the top end of the upper reciprocating shaft and the lower reciprocating shaft in the freezing chamber.
By adopting the technical scheme, when the sample grinding device is used, a sample in the freezing chamber is frozen through the refrigerating device, then the vacuum generating device is used for pumping vacuum in the vacuum chamber and the freezing chamber, and finally the reciprocating device drives the sample tube to reciprocate at high frequency to finish sample grinding. After the sample is set, freezing and grinding are finished in the freezing chamber, the cold quantity loss is reduced, the sample is ground after being vacuumized, air is not blocked during high-frequency reciprocating motion, the noise is reduced, the cold quantity loss of the sample is small, the stability of the sample before and after grinding is ensured, the grinding efficiency is improved, and the sample with lower fineness can be obtained.
Further, the reciprocating device comprises a vacuum motor, a rotary disc, a connecting rod, a linear bearing, an upper reciprocating shaft, a lower reciprocating shaft and a supporting seat, wherein the rotary disc is installed on a rotating shaft of the vacuum motor, one end of the connecting rod is eccentrically connected to the rotary disc, the other end of the connecting rod is connected to the upper reciprocating shaft and the lower reciprocating shaft, the upper reciprocating shaft and the lower reciprocating shaft are arranged in the linear bearing in a penetrating mode, and the linear bearing is installed on the supporting seat below the freezing chamber.
By adopting the preferable scheme, the structure is simple, and high-frequency reciprocating oscillation can be stably output.
Furthermore, a sealing flange plate which is expanded outwards is arranged at the position, above the linear bearing, of the upper reciprocating shaft and the lower reciprocating shaft, a wave-shaped sealing washer is arranged at the bottom of the freezing chamber, an inner opening of the wave-shaped sealing washer is positioned right above the sealing flange plate, an electromagnetic magnet is arranged at the inner opening of the wave-shaped sealing washer, and a reset pressure spring is arranged between the lower surface of the wave-shaped sealing washer and the supporting seat; when the electromagnetic magnet is electrified, attraction force is generated between the electromagnetic magnet and the sealing flange plate, the lower surface of the inner opening of the wavy sealing washer is attached to the sealing flange plate, and sealing isolation is formed between the freezing chamber and the vacuum chamber; after the electromagnetic magnet loses power, the reset pressure spring drives the inner opening of the wave-shaped sealing washer and the electromagnetic magnet to reset upwards to be separated from the sealing flange plates of the upper reciprocating shaft and the lower reciprocating shaft, and the wave-shaped sealing washer and the electromagnetic magnet do not interfere with the upper reciprocating shaft and the lower reciprocating shaft during grinding.
By adopting the preferred scheme, when the grinding is not carried out, the air leakage of the gap between the upper reciprocating shaft and the lower reciprocating shaft and the linear bearing can be effectively avoided, the reliable sealing is formed between the freezing chamber and the vacuum chamber, the respective vacuumizing of the freezing chamber and the vacuum chamber is conveniently realized, and the efficient freezing and vacuumizing optimization program is realized in a matching manner; when the grinding is started, the high-frequency reciprocating oscillation of the upper reciprocating shaft and the lower reciprocating shaft can not be interfered, so that the grinding efficiency is improved.
Furthermore, a second vacuumizing interface is arranged on the wall body of the freezing chamber; the vacuum generating device comprises a vacuum pump, a first vacuumizing interface of the vacuum chamber is connected to a suction port of the vacuum pump through a pipeline and a first control valve, and a second vacuumizing interface of the freezing chamber is connected to the suction port of the vacuum pump through a pipeline and a second control valve.
By adopting the preferable scheme, the vacuum pump can be comprehensively utilized to realize the cooperative operation of vacuumizing the freezing chamber and the vacuum chamber.
Further, the vacuum degree detection device also comprises a first air pressure detection device for detecting the vacuum degree in the vacuum chamber and a second air pressure detection device for detecting the vacuum degree in the freezing chamber.
Adopt above-mentioned preferred scheme, be convenient for detect the real-time vacuum degree of freezing chamber and vacuum chamber to realize the accurate control to the extraction vacuum degree.
Furthermore, the refrigerating device comprises a liquid nitrogen refrigerating device and a heat pump refrigerating system, the liquid nitrogen refrigerating device comprises a liquid nitrogen tank, a third control valve and a low-temperature pump, a plurality of liquid nitrogen ejection outlets are formed in the freezing chamber, and an outlet of the liquid nitrogen tank is connected to the liquid nitrogen ejection outlets of the freezing chamber through a pipeline, the third control valve and the low-temperature pump; the heat pump refrigeration system comprises a compressor, a gas-liquid separator, an evaporator coil, an expansion valve and a condenser which are sequentially connected in series through pipelines, wherein the evaporator coil surrounds the periphery of the freezing chamber, the evaporator coil is located in the vacuum chamber, and the compressor, the gas-liquid separator, the expansion valve and the condenser are all located outside the vacuum chamber.
Further, a temperature sensor for detecting the temperature in the freezing chamber is also included.
By adopting the preferable scheme, the heat pump refrigerating system can pre-cool the sample before grinding, so that the consistency of the temperature condition of the sample before freezing liquid nitrogen is ensured, the ground sample is conveniently kept cold after grinding, and the use of liquid nitrogen resources is saved; the liquid nitrogen refrigerating device can provide extremely low freezing temperature for the sample so as to improve the grinding efficiency of the tough sample difficult to grind and ensure that the sample with lower fineness is obtained.
Further, still include the interim energy storage ware of nitrogen gas, the interim energy storage ware of nitrogen gas is connected to in the freezing chamber through pipeline, fourth control valve and air pump.
By adopting the preferable scheme, the liquid nitrogen volatile gas is conveniently and comprehensively utilized, and the energy consumption of the grinding device is reduced.
A vacuum freeze grinding method comprising the steps of:
step 2, refrigerating the freezing chamber through a refrigerating device to freeze a sample; vacuumizing the vacuum chamber and the freezing chamber by a vacuum generating device;
and 3, starting the reciprocating motion device to grind.
By adopting the technical scheme of the invention, after the sample is set, freezing and grinding are finished in the freezing chamber, so that the loss of cold energy is reduced, the sample is ground after being vacuumized, no air is blocked during high-frequency reciprocating motion, the noise is reduced, the loss of the cold energy of the sample is small, the temperature of the sample can be stably kept in a precise low-temperature range, and the stability of the characteristics of the sample before and after grinding is ensured.
Further, step 2 comprises:
step 21, electrifying the electromagnetic magnet, enabling the lower surface of the inner opening of the wave-shaped sealing washer to be attached to the sealing flange plate, and forming sealing isolation between the freezing chamber and the vacuum chamber;
step 22, starting a vacuum pump and a first control valve, vacuumizing a vacuum chamber until the air pressure value of the vacuum chamber detected by a first air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the first control valve, wherein the first set vacuum value is 0.1-5 Pa; simultaneously starting a heat pump refrigerating system to refrigerate the freezing cavity, and starting the step 23 after the temperature of the freezing cavity detected by the temperature sensor reaches a first set temperature value, wherein the first set temperature value is-4 ℃ to-16 ℃;
step 23, after the temperature of the freezing chamber reaches a first set temperature value, opening a first control valve and a second control valve to communicate the freezing chamber with the vacuum chamber, performing air pressure balance of the two chambers, then closing the first control valve, opening a vacuum pump and a second control valve, vacuumizing the freezing chamber until the air pressure value of the freezing chamber detected by a second air pressure detection device reaches a second set vacuum value, and then closing the second control valve to start step 24, wherein the second set vacuum value is 20-100 Pa; after the second control valve is closed, opening the first control valve to continue vacuumizing the vacuum chamber until the air pressure value of the vacuum chamber detected by the first air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the first control valve;
step 24, opening a third control valve and a cryogenic pump, feeding liquid nitrogen with a set flow into the freezing chamber, and preserving heat for 5-20 seconds; then, a fourth control valve and a gas pump are started, nitrogen in the freezing chamber is pumped into the temporary nitrogen accumulator until the air pressure value of the freezing chamber detected by the second air pressure detection device reaches a third set vacuum value, and then the fourth control valve and the gas pump are closed, wherein the third set vacuum value is 200-300 Pa;
step 25, repeating the step 24 according to the set cyclic nitrogen addition numerical value;
step 26, starting a vacuum pump and a second control valve, vacuumizing the freezing chamber until the air pressure value of the vacuum chamber detected by the second air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the second control valve;
step 27, when the electromagnetic magnet loses power, the reset pressure spring drives the inner opening of the wave-shaped sealing washer and the electromagnetic magnet to reset upwards to be separated from the sealing flange plates of the upper reciprocating shaft and the lower reciprocating shaft, and the reciprocating motion device is started to grind a sample;
28, after grinding is finished, electrifying the electromagnetic magnet, enabling the lower surface of the inner opening of the wavy sealing washer to be attached to the sealing flange plate, and forming sealing isolation between the freezing chamber and the vacuum chamber; and opening a fourth control valve and an air pump, pumping the nitrogen in the temporary nitrogen accumulator into the freezing chamber until the air pressure value of the freezing chamber detected by the second air pressure detection device reaches 0.1MPa, and then closing the fourth control valve and the air pump.
By adopting the preferable scheme, the vacuumizing of the vacuum chamber and the pre-cooling and freezing of the freezing chamber are synchronously matched, so that the obtaining speed of high vacuum and low freezing temperature before grinding is improved; the liquid nitrogen is subjected to cyclic refrigeration in multiple steps, so that the utilization rate of the liquid nitrogen can be improved, a sample can be frozen below 150 ℃, the fineness can be obtained, the grinding time can be greatly shortened, and the grinding efficiency can be improved; the temporary nitrogen accumulator can comprehensively utilize nitrogen volatilized in the freezing process, fully utilizes cold quantity, and keeps the sample cold and fresh after grinding.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a perspective view of one embodiment of the present invention;
FIG. 2 is a top view of one embodiment of the present invention;
FIG. 3 is a cross-sectional view taken along line A-A of FIG. 2;
FIG. 4 is a cross-sectional view of another embodiment of the present invention;
FIG. 5 is a partial enlarged view of FIG. 4 at B;
fig. 6 is a schematic view of the refrigeration and evacuation principle of the present invention.
Names of corresponding parts represented by numerals and letters in the drawings:
10-a vacuum chamber; 20-a freezing chamber; 30-a reciprocating device; 31-a vacuum motor; 32-a turntable; 33-a connecting rod; 34-a linear bearing; 35-up and down reciprocating shaft; 351-sealing flange; 36-a support base; 40-upper cover; 51-a wave-shaped sealing gasket; 52-electromagnet; 53-return compression spring; 61-a vacuum pump; 62-a first control valve; 63-a second control valve; 71-liquid nitrogen tank; 72-a third control valve; 73-a cryopump; 81-compressor; 82-a gas-liquid separator; 83-evaporator coil; 84-an expansion valve; 85-a condenser; 91-nitrogen temporary accumulator; 92-a fourth control valve; 93-air pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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 to 3, a vacuum freeze-grinding apparatus includes:
a vacuum chamber 10, wherein a vacuumizing interface is arranged on the wall body of the vacuum chamber 10;
a vacuum generating device for drawing a vacuum to the vacuum chamber;
a freezing chamber 20 disposed within the vacuum chamber 10;
a refrigerating device for providing a cold source to the freezing chamber, a main machine of the refrigerating device being located outside the vacuum chamber 10;
a reciprocating device 30 installed in the vacuum chamber 10, wherein a vertical reciprocating shaft 35 of the reciprocating device 30 is inserted into the freezing chamber from the bottom of the freezing chamber 20;
the adapter is used for placing a sample tube and is arranged at the top end of the upper reciprocating shaft and the lower reciprocating shaft in the freezing chamber.
The beneficial effect of adopting above-mentioned technical scheme is: during the use, the sample of freezing cavity is frozen through refrigerating plant earlier, then draws the vacuum in vacuum chamber and the freezing cavity through vacuum generating device, and reciprocating motion device drives sample tube high frequency reciprocating motion at last accomplishes the sample and grinds. After the sample is arranged, freezing, vacuumizing and grinding are all completed in the freezing chamber, the loss of cold energy is reduced, the sample is ground again after vacuumizing, air is not blocked during high-frequency reciprocating motion, noise is reduced, the loss of the cold energy of the sample is small, the sample can be stably kept in an accurate low-temperature range, and the stability of the sample before and after grinding is ensured.
As shown in fig. 3, in another embodiment of the present invention, the reciprocating device 30 includes a vacuum motor 31, a turntable 32, a connecting rod 33, a linear bearing 34, and an up-down reciprocating shaft 35, wherein the turntable 32 is mounted on a rotating shaft of the vacuum motor 31, one end of the connecting rod 33 is eccentrically connected to the turntable 32, the other end of the connecting rod 33 is connected to the up-down reciprocating shaft 35, the up-down reciprocating shaft 35 is inserted into the linear bearing 34, and the linear bearing 34 is mounted on a supporting base 36 below the freezing chamber. The beneficial effect of adopting above-mentioned technical scheme is: simple structure can stably output high-frequency reciprocating oscillation.
As shown in fig. 4 to 5, in other embodiments of the present invention, the upper and lower reciprocating shafts 35 are provided with an outwardly expanding sealing flange 351 at a position above the linear bearing, a wave-shaped sealing washer 51 is provided at the bottom of the freezing chamber 20, an inner opening of the wave-shaped sealing washer 51 is located right above the sealing flange 351, an electromagnetic magnet 52 is provided at the inner opening of the wave-shaped sealing washer 51, and a return pressure spring 53 is further provided between the lower surface of the wave-shaped sealing washer and the supporting base 36; when the electromagnet 52 is electrified, suction force is generated between the electromagnet 52 and the sealing flange 351, the lower surface of the inner opening of the wavy sealing washer 51 is attached to the sealing flange 351, sealing isolation is formed between the freezing chamber and the vacuum chamber, the wave section of the wavy sealing washer can buffer expansion caused by thermal expansion and contraction caused by cold contraction, and in order to improve the sealing isolation performance, an elastic rubber layer is arranged on the lower surface of the inner opening of the wavy sealing washer 51 and the upper surface of the sealing flange 351; after the electromagnet 52 loses power, the reset pressure spring 53 drives the inner opening of the wave-shaped sealing washer and the electromagnet 52 to reset upwards to be separated from the sealing flange 351 of the upper reciprocating shaft and the lower reciprocating shaft, and the wave-shaped sealing washer 51 and the electromagnet 52 are not interfered with the upper reciprocating shaft 35 during grinding. The beneficial effect of adopting above-mentioned technical scheme is: when the grinding is not carried out, the air leakage of the gap between the upper reciprocating shaft and the lower reciprocating shaft and the linear bearing can be effectively avoided, reliable sealing is formed between the freezing chamber and the vacuum chamber, the freezing chamber and the vacuum chamber can be conveniently and respectively vacuumized, and the efficient freezing and vacuumizing optimization program can be realized in a matching manner; when the grinding is started, the high-frequency reciprocating oscillation of the upper reciprocating shaft and the lower reciprocating shaft can not be interfered, so that the grinding efficiency is improved.
In other embodiments of the present invention, as shown in fig. 6, a second evacuation port is provided on the wall of the freezing chamber 20; the vacuum generating device comprises a vacuum pump 61, a first evacuation port of the vacuum chamber 10 is connected to an inlet port of the vacuum pump 61 via a pipe and a first control valve 62, and a second evacuation port of the freezing chamber 20 is connected to an inlet port of the vacuum pump 61 via a pipe and a second control valve 63. The beneficial effect of adopting above-mentioned technical scheme is: the vacuum pump can be comprehensively utilized to realize the cooperative operation of vacuumizing the freezing chamber and the vacuum chamber.
In other embodiments of the present invention, a first air pressure detecting device for detecting the degree of vacuum within the vacuum chamber 10 and a second air pressure detecting device for detecting the degree of vacuum within the freezing chamber 20 are further included. The beneficial effect of adopting above-mentioned technical scheme is: the real-time vacuum degree of freezing cavity and vacuum chamber is convenient for detect to the realization is to the accurate control of extraction vacuum degree.
In other embodiments of the present invention, as shown in fig. 6, the refrigerating apparatus includes a liquid nitrogen refrigerating apparatus and a heat pump refrigerating system, the liquid nitrogen refrigerating apparatus includes a liquid nitrogen tank 71, a third control valve 72 and a cryogenic pump 73, a plurality of liquid nitrogen discharge ports are provided in the freezing chamber 20, an outlet of the liquid nitrogen tank 71 is connected to the liquid nitrogen discharge port of the freezing chamber 20 via a pipeline, the third control valve 72 and the cryogenic pump 73; the heat pump refrigeration system comprises a compressor 81, a gas-liquid separator 82, an evaporator coil 83, an expansion valve 84 and a condenser 85 which are connected in series in sequence through pipelines, wherein the evaporator coil 83 surrounds the periphery of the freezing chamber 20, the evaporator coil 83 is positioned in the vacuum chamber 10, and the compressor 81, the gas-liquid separator 82, the expansion valve 84 and the condenser 85 are all positioned outside the vacuum chamber 10. A temperature sensor for sensing the temperature within the freezing chamber 20 is also included, and multiple temperature sensors may be used to collect the temperature in different areas of the freezing chamber in order to improve the accuracy of the temperature collection. The beneficial effect of adopting above-mentioned technical scheme is: the sample can be precooled before grinding through the heat pump refrigerating system, the consistency of the temperature condition of the sample before freezing of liquid nitrogen is ensured, the ground sample can be conveniently kept cold after grinding, and the use of liquid nitrogen resources is saved; the liquid nitrogen refrigerating device can provide extremely low freezing temperature for the sample so as to improve the grinding efficiency of the tough sample difficult to grind and ensure that the sample with lower fineness is obtained.
As shown in fig. 6, in other embodiments of the present invention, a nitrogen temporary storage 91 is further included, and the nitrogen temporary storage 91 is connected to the freezing chamber 20 through a pipe, a fourth control valve 92, and an air pump 93. The fourth control valve 92 can be used for inflating and deflating the nitrogen temporary energy storage 91 by means of one air pump 93, the fourth control valve 92 can be controlled by a two-position four-way valve or by integrated cooperation of a plurality of valve groups, and a specific air path connection method can be obtained from the prior art and is not the creation point of the application. The beneficial effect of adopting above-mentioned technical scheme is: the comprehensive utilization of the liquid nitrogen volatile gas is facilitated, and the energy consumption of the grinding device is reduced.
A vacuum freeze grinding method comprising the steps of:
step 2, refrigerating the freezing chamber through a refrigerating device to freeze a sample; vacuumizing the vacuum chamber and the freezing chamber by a vacuum generating device;
and 3, starting the reciprocating motion device to grind.
In other embodiments of the invention, step 2 comprises, in sequence:
step 21, electrifying the electromagnetic magnet, enabling the lower surface of the inner opening of the wave-shaped sealing washer to be attached to the sealing flange plate, and forming sealing isolation between the freezing chamber and the vacuum chamber;
step 22, starting a vacuum pump and a first control valve, vacuumizing a vacuum chamber until the air pressure value of the vacuum chamber detected by a first air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the first control valve, wherein the first set vacuum value (absolute pressure value) is 0.1-5 Pa; simultaneously starting a heat pump refrigerating system to refrigerate the freezing cavity, and starting the step 23 after the temperature of the freezing cavity detected by the temperature sensor reaches a first set temperature value, wherein the first set temperature value is-4 ℃ to-16 ℃;
step 23, after the temperature of the freezing chamber reaches a first set temperature value, opening a first control valve and a second control valve to communicate the freezing chamber with the vacuum chamber, performing air pressure balance of the two chambers, then closing the first control valve, opening a vacuum pump and a second control valve, vacuumizing the freezing chamber until the air pressure value of the freezing chamber detected by a second air pressure detection device reaches a second set vacuum value, and then closing the second control valve to start step 24, wherein the second set vacuum value (absolute pressure value) is 20-100 Pa; after the second control valve is closed, opening the first control valve to continue vacuumizing the vacuum chamber until the air pressure value of the vacuum chamber detected by the first air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the first control valve;
step 24, opening a third control valve and a cryogenic pump, feeding liquid nitrogen with a set flow into the freezing chamber, and preserving heat for 5-20 seconds; then, a fourth control valve and a gas pump are started, nitrogen in the freezing chamber is pumped into the temporary nitrogen accumulator until the air pressure value of the freezing chamber detected by the second air pressure detection device reaches a third set vacuum value, and then the fourth control valve and the gas pump are closed, wherein the third set vacuum value (absolute pressure value) is 200-300 Pa;
step 25, repeating step 24 according to the set value of the cyclic nitrogen addition times, wherein the cyclic nitrogen addition times are at least 2 times, preferably 3-5 times;
step 26, starting a vacuum pump and a second control valve, vacuumizing the freezing chamber until the air pressure value of the vacuum chamber detected by the second air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the second control valve;
step 27, when the electromagnet loses power, the reset pressure spring drives the inner opening of the wavy sealing washer and the electromagnet to reset upwards to be separated from the sealing flange of the upper reciprocating shaft and the lower reciprocating shaft, and the reciprocating device is started to grind a sample;
28, after grinding is finished, electrifying the electromagnetic magnet, enabling the lower surface of the inner opening of the wavy sealing washer to be attached to the sealing flange plate, and forming sealing isolation between the freezing chamber and the vacuum chamber; and opening a fourth control valve and an air pump, pumping the nitrogen in the temporary nitrogen accumulator into the freezing chamber until the air pressure value of the freezing chamber detected by the second air pressure detection device reaches 0.1MPa, and then closing the fourth control valve and the air pump.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered in the scope of the present invention.
Claims (10)
1. A vacuum freeze grinding apparatus, comprising:
the vacuum chamber is provided with a first vacuumizing interface on a wall body;
the freezing chamber is arranged in the vacuum chamber, a discharge hole is formed above the freezing chamber, and a sealing cover capable of being opened and closed is arranged at the discharge hole;
a vacuum generating device for drawing a vacuum to the vacuum chamber and the freezing chamber;
the refrigerating device is used for providing a cold source for the freezing chamber, and a main machine of the refrigerating device is positioned outside the vacuum chamber;
the reciprocating device is arranged in the vacuum chamber, and an upper reciprocating shaft and a lower reciprocating shaft of the reciprocating device penetrate through the freezing chamber from the bottom of the freezing chamber;
the adapter is used for placing a sample tube and is arranged at the top end of the upper reciprocating shaft and the lower reciprocating shaft in the freezing chamber.
2. The vacuum freeze grinding device according to claim 1, wherein the reciprocating device comprises a vacuum motor, a turntable, a connecting rod, a linear bearing, an up-down reciprocating shaft and a support seat, the turntable is mounted on a rotating shaft of the vacuum motor, one end of the connecting rod is eccentrically connected to the turntable, the other end of the connecting rod is connected to the up-down reciprocating shaft, the up-down reciprocating shaft is inserted into the linear bearing, and the linear bearing is mounted on the support seat below the freezing chamber.
3. The vacuum freeze grinding device according to claim 2, wherein the upper and lower reciprocating shafts have outwardly expanded sealing flanges at positions above the linear bearings, a wavy sealing gasket is arranged at the bottom of the freezing chamber, an inner opening of the wavy sealing gasket is positioned right above the sealing flanges, an electromagnetic magnet is arranged at the inner opening of the wavy sealing gasket, and a reset pressure spring is further arranged between the lower surface of the wavy sealing gasket and the supporting seat; when the electromagnetic magnet is electrified, attraction force is generated between the electromagnetic magnet and the sealing flange plate, the lower surface of the inner opening of the wavy sealing washer is attached to the sealing flange plate, and sealing isolation is formed between the freezing chamber and the vacuum chamber; after the electromagnetic magnet loses power, the reset pressure spring drives the inner opening of the wave-shaped sealing washer and the electromagnetic magnet to reset upwards to be separated from the sealing flange plates of the upper reciprocating shaft and the lower reciprocating shaft, and the wave-shaped sealing washer and the electromagnetic magnet do not interfere with the upper reciprocating shaft and the lower reciprocating shaft during grinding.
4. The vacuum freeze grinding apparatus of claim 3, wherein the freeze chamber wall has a second evacuation port; the vacuum generating device comprises a vacuum pump, a first vacuumizing interface of the vacuum chamber is connected to a suction port of the vacuum pump through a pipeline and a first control valve, and a second vacuumizing interface of the freezing chamber is connected to the suction port of the vacuum pump through a pipeline and a second control valve.
5. The vacuum freeze grinding apparatus of claim 4, further comprising a first air pressure detecting device for detecting a degree of vacuum in the vacuum chamber and a second air pressure detecting device for detecting a degree of vacuum in the freeze chamber.
6. The vacuum freeze-grinding apparatus according to claim 1, wherein the refrigerating apparatus includes a liquid nitrogen refrigerating apparatus and a heat pump refrigerating system, the liquid nitrogen refrigerating apparatus includes a liquid nitrogen tank, a third control valve and a cryogenic pump, a plurality of liquid nitrogen ejection ports are provided in the freezing chamber, and an outlet of the liquid nitrogen tank is connected to the liquid nitrogen ejection port of the freezing chamber through a pipeline, the third control valve and the cryogenic pump; the heat pump refrigeration system comprises a compressor, a gas-liquid separator, an evaporator coil, an expansion valve and a condenser which are sequentially connected in series through pipelines, wherein the evaporator coil surrounds the periphery of the freezing chamber, the evaporator coil is located in the vacuum chamber, and the compressor, the gas-liquid separator, the expansion valve and the condenser are all located outside the vacuum chamber.
7. The vacuum cryogrinding apparatus of claim 6, further comprising a temperature sensor for detecting a temperature within the freezing chamber.
8. The vacuum freeze grinding apparatus of claim 7, further comprising a nitrogen temporary accumulator connected to the freezing chamber via a line, a fourth control valve, and a gas pump.
9. A vacuum freeze-grinding method using the vacuum freeze-grinding apparatus according to any one of claims 1 to 8, comprising the steps of:
step 1, mounting an adapter provided with a sample tube on an upper reciprocating shaft and a lower reciprocating shaft of a reciprocating motion device, and closing a sealing cover of a freezing chamber;
step 2, refrigerating the freezing chamber through a refrigerating device to freeze a sample; vacuumizing the vacuum chamber and the freezing chamber by a vacuum generating device;
and 3, starting the reciprocating motion device to grind.
10. The vacuum freeze-grinding method according to claim 9, wherein,
the step 2 comprises the following steps:
step 21, electrifying the electromagnetic magnet, enabling the lower surface of the inner opening of the wave-shaped sealing washer to be attached to the sealing flange plate, and forming sealing isolation between the freezing chamber and the vacuum chamber;
step 22, starting a vacuum pump and a first control valve, vacuumizing a vacuum chamber until the air pressure value of the vacuum chamber detected by a first air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the first control valve, wherein the first set vacuum value is 0.1-5 Pa; simultaneously starting a heat pump refrigerating system to refrigerate the freezing cavity, and starting the step 23 after the temperature of the freezing cavity detected by the temperature sensor reaches a first set temperature value, wherein the first set temperature value is-4 ℃ to-16 ℃;
step 23, after the temperature of the freezing chamber reaches a first set temperature value, opening a first control valve and a second control valve to communicate the freezing chamber with the vacuum chamber, performing air pressure balance of the two chambers, then closing the first control valve, opening a vacuum pump and a second control valve, vacuumizing the freezing chamber until the air pressure value of the freezing chamber detected by a second air pressure detection device reaches a second set vacuum value, and then closing the second control valve to start step 24, wherein the second set vacuum value is 20-100 Pa; after the second control valve is closed, opening the first control valve to continue vacuumizing the vacuum chamber until the air pressure value of the vacuum chamber detected by the first air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the first control valve;
step 24, opening a third control valve and a cryogenic pump, feeding liquid nitrogen with a set flow into the freezing chamber, and preserving heat for 5-20 seconds; then, a fourth control valve and a gas pump are started, nitrogen in the freezing chamber is pumped into the temporary nitrogen accumulator until the air pressure value of the freezing chamber detected by the second air pressure detection device reaches a third set vacuum value, and then the fourth control valve and the gas pump are closed, wherein the third set vacuum value is 200-300 Pa;
step 25, repeating the step 24 according to the set cyclic nitrogen addition numerical value;
step 26, starting a vacuum pump and a second control valve, vacuumizing the freezing chamber until the air pressure value of the vacuum chamber detected by the second air pressure detection device reaches a first set vacuum value, and then closing the vacuum pump and the second control valve;
step 27, when the electromagnetic magnet loses power, the reset pressure spring drives the inner opening of the wave-shaped sealing washer and the electromagnetic magnet to reset upwards to be separated from the sealing flange plates of the upper reciprocating shaft and the lower reciprocating shaft, and the reciprocating motion device is started to grind a sample;
28, after grinding is finished, electrifying the electromagnetic magnet, enabling the lower surface of the inner opening of the wavy sealing washer to be attached to the sealing flange plate, and forming sealing isolation between the freezing chamber and the vacuum chamber; and opening a fourth control valve and an air pump, pumping the nitrogen in the temporary nitrogen accumulator into the freezing chamber until the air pressure value of the freezing chamber detected by the second air pressure detection device reaches 0.1MPa, and then closing the fourth control valve and the air pump.
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