CN110736568B - Large-scale water triple-point bottle ice sleeve freezing device and method - Google Patents

Large-scale water triple-point bottle ice sleeve freezing device and method Download PDF

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Publication number
CN110736568B
CN110736568B CN201911071544.6A CN201911071544A CN110736568B CN 110736568 B CN110736568 B CN 110736568B CN 201911071544 A CN201911071544 A CN 201911071544A CN 110736568 B CN110736568 B CN 110736568B
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temperature
low
triple point
water triple
point bottle
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CN110736568A (en
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刘颖
张雯
张秋泉
冯黎
罗涵
梁志华
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Chongqing Academy of Metrology and Quality Inspection
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01KMEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K15/00Testing or calibrating of thermometers
    • G01K15/002Calibrated temperature sources, temperature standards therefor

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Abstract

The invention discloses a large-scale water triple point bottle ice sleeve freezing device, which comprises a low-temperature tank and a freezing device, wherein the low-temperature tank is provided with a freezing chamber; the low-temperature tank comprises a tank shell, a supporting sheet, a bracket, a refrigerating system, a heating system, a circulating system and a temperature control system; the supporting sheet is fixedly arranged on the outer wall of the groove shell and used for placing the freezer; the bracket is used for placing a water triple point bottle and soaking the bottle in a low-temperature medium contained in the tank shell; the refrigerating system is used for providing a cold source for the low-temperature tank, and the heating system is used for providing a heat source for the low-temperature tank; the circulating system comprises a motor and a stirring paddle, the temperature control system comprises a temperature controller and a temperature sensor, the freezing device comprises a heat conduction rod and a liquid containing cup, the liquid containing cup is used for containing liquid nitrogen, the heat conduction rod is vertically inserted into a water triple point bottle thermometer well, and the top of the heat conduction rod is welded with stainless steel of the liquid containing cup. The invention also discloses a large water triple point bottle ice sleeve freezing method. The device and the method for freezing the ice sleeve have low requirement on operators, high efficiency, uniform thickness of the ice sleeve and long service life.

Description

Large-scale water triple-point bottle ice sleeve freezing device and method
Technical Field
The invention relates to a device and a method for freezing three-phase point bottle ice in a sleeving manner, in particular to a device and a method for freezing large-scale water three-phase point bottle ice in a sleeving manner.
Background
The water triple point is the only reference point of Kelvin thermodynamic temperature and is also an important defined fixed point in ITS-90 international temperature scale, and has very important significance in thermodynamic temperature measurement, international temperature scale recurrence and actual temperature measurement. The water triple point is reproduced by freezing an ice sleeve in a water triple point container. According to the size, the water three-phase point bottle can be divided into a small water three-phase point bottle and a large water three-phase point bottle, the small water three-phase point bottle is mainly used for detecting an industrial platinum resistance thermometer, and the large water three-phase point bottle is mainly used for detecting a standard platinum resistance thermometer. The method for freezing the ice sleeve of the large water three-phase point bottle commonly used at present is a liquid nitrogen freezing method, and the method comprises the steps of firstly putting the water three-phase point bottle into a Dewar bottle filled with crushed ice for precooling for 4-5 hours, then manually and slowly filling liquid nitrogen into a thermometer trap of the water three-phase point bottle, simultaneously inserting a glass rod with a cotton ball on the top into the thermometer trap to limit the position where the liquid nitrogen stays, and diffusing a cold source by pulling up and down to ensure that the obtained ice sleeve has a smooth appearance and uniform thickness. The method has higher technical requirements on operators, is easy to freeze the ice sleeve with uneven thickness from top to bottom if the operators do not master the ice sleeve well, and has long time consumption and lower efficiency in the whole process from preparation to freezing.
Disclosure of Invention
The invention provides a device and a method for freezing a large-scale water three-phase point bottle ice sleeve, and solves the technical problems that the existing freezing method for the large-scale water three-phase point bottle ice sleeve has higher technical requirements on operators, longer freezing time and lower efficiency.
In order to solve the technical problems, the invention adopts the following technical scheme:
a large-scale water triple point bottle ice sleeve freezing device comprises a low-temperature tank and a freezer;
the low-temperature tank comprises a tank shell, a supporting sheet, a bracket, a refrigerating system, a heating system, a circulating system and a temperature control system;
the supporting sheet is of a circular ring structure, is fixedly arranged on the outer wall of the groove shell and is used for placing the freezer;
the bracket is used for placing a water triple point bottle and is soaked in a low-temperature medium contained in the tank shell;
the refrigeration system is used for providing a cold source for the low-temperature tank and comprises a compressor and an evaporator; the compressor is arranged below the tank shell, the evaporator is arranged in the tank shell, and the compressor is connected with the evaporator through a refrigerant circulating pipeline;
the heating system is used for providing a heat source for the low-temperature tank, and the heating system is a heating resistance wire arranged in the tank shell;
the circulating system comprises a motor and a stirring paddle, the stirring paddle is immersed in the low-temperature medium contained in the tank shell, the stirring paddle is driven by a power output shaft of the motor, the low-temperature medium circularly flows from bottom to top through the rotation of the stirring paddle, and the uniformity of a temperature field in the whole low-temperature tank is ensured;
the temperature control system comprises a temperature controller and a temperature sensor, the temperature sensor collects the temperature of the low-temperature medium contained in the tank shell and feeds the measured temperature back to the temperature controller, the output power of the cold source and the heat source is adjusted through the temperature controller, and then the temperature of the low-temperature medium contained in the tank shell is adjusted;
the freezing device comprises a heat conducting rod and a liquid containing cup, wherein the heat conducting rod is a hollow copper rod; the liquid containing cup is used for containing liquid nitrogen and is composed of a three-layer structure, wherein the innermost layer is made of stainless steel, the stainless steel is wrapped by a heat insulation material, and the outermost layer is made of a plastic material; the liquid containing cup is arranged above the support, the heat conducting rod is vertically inserted into the thermometer well of the water triple point bottle, and the top of the heat conducting rod is welded with the stainless steel of the liquid containing cup.
In a preferred embodiment of the present invention, a baffle is disposed between the stirring paddle and the support, and a gap is formed between the bottom of the baffle and the bottom of the tank shell.
Meanwhile, the invention also discloses a large-scale water three-phase point bottle ice sleeve freezing method, wherein the method adopts the large-scale water three-phase point bottle ice sleeve freezing device, and the method comprises the following steps:
1) before the freezing process is started, the low-temperature tank is started, and the working temperature of the low-temperature tank is stabilized at 0 ℃;
2) placing a water triple point bottle on a support in a low-temperature tank for precooling for 30min, then inserting a heat conducting rod of a freezer into a thermometer well of the water triple point bottle, filling alcohol into the thermometer well of the water triple point bottle, injecting liquid nitrogen into a liquid containing cup of the freezer, taking away heat through evaporation of the liquid nitrogen, taking out the freezer after freezing for 10min, and placing the freezer on a support plate on a tank shell;
3) taking out the water triple point bottle, manually shaking the bottle to enable ice crystals to appear in the water triple point bottle to form crystal nuclei, and rotating the water triple point bottle to enable the crystal nuclei to be uniformly distributed in the water triple point bottle;
4) putting the water triple point bottle on a support in a low-temperature tank again, filling alcohol in a thermometer well of the water triple point bottle again, putting a heat conducting rod of the freezer into the thermometer well of the water triple point bottle, keeping liquid nitrogen in a liquid containing cup of the freezer all the time in the freezing process, continuously freezing, starting to form an ice sleeve along the inner wall of the thermometer well of the water triple point bottle towards the outer wall, taking out the water triple point bottle after freezing is restricted for 2min, and rotating the ice sleeve to prevent an ice bridge from being generated;
5) and (3) placing the water triple point bottle on a support in a low-temperature groove, placing a heat conducting rod of the freezing device in a thermometer well of the water triple point bottle to continue freezing, and repeating the operation until the thickness of the frozen ice sleeve reaches the required thickness.
The invention has the technical effects that: the device and the method for freezing the ice sleeve have low requirement on operators, high efficiency, uniform thickness of the ice sleeve and long service life.
Drawings
Fig. 1 shows a large scale water triple point bottle ice sleeve freezing device.
In the figure, 1-tank enclosure; 2-a support sheet; 3, a bracket; 4, a compressor; 5-an evaporator; 6-heating resistance wires; 7-stirring paddle; 8, a motor; 9-a baffle plate; 10-heat conducting rod; 11-liquid containing cup; 12-water triple point bottle; 13-water triple point bottle thermometer trap.
Detailed Description
The invention is described in further detail below with reference to the figures and the detailed description.
As shown in fig. 1, a large scale water triple point bottle ice sleeve freezing device comprises a low temperature tank and a freezer.
The low-temperature tank comprises a tank shell 1, a support sheet 2, a support 3, a refrigerating system, a heating system, a circulating system and a temperature control system.
The supporting sheet 2 is of a circular ring structure, and the supporting sheet 2 is fixedly arranged on the outer wall of the groove shell 1 and used for placing a freezer. In this embodiment, the outer wall of the tank case 1 is provided with two support pieces 2 by welding, the two support pieces 2 vertically correspond to each other, and the center holes of the two support pieces 2 vertically correspond to each other. When the freezer is placed, the heat conducting rod 10 of the freezer only needs to penetrate through the central holes of the two support sheets 2 from top to bottom, and the liquid containing cup 11 of the freezer is placed on the uppermost support sheet 2.
The bracket 3 is used for placing a water triple point bottle 12, the bracket 3 is soaked in a low-temperature medium contained in the tank shell 1, and the position of the bracket 3 in the tank shell 1 can be moved. The bracket 3 can also be taken out, and different sizes of brackets 3 can be designed aiming at different types of water triple point bottles 12.
The refrigeration system is used to provide a cold source to the cryogenic tank and comprises a compressor 4 and an evaporator 5. The compressor 4 is arranged below the tank shell 1, the evaporator 5 is arranged in the tank shell 1, the compressor 4 is connected with the evaporator 5 through a refrigerant circulating pipeline, the compressor 4 and the evaporator 5 are adopted for refrigeration, the principle of the refrigeration is the same as that of the refrigeration of a refrigerator, and the details are not repeated. Of course, the cold source is provided for the low-temperature tank, and the cold source can be refrigerated by a compressor or a semiconductor.
The heating system is used for providing a heat source for the low-temperature tank and is a heating resistance wire 6 arranged in the tank shell 1.
The circulating system comprises a motor 8 and a stirring paddle 7, the stirring paddle 7 is immersed in the low-temperature medium contained in the tank shell 1, the stirring paddle 7 is driven by a power output shaft of the motor 8, the low-temperature medium circularly flows from bottom to top through the rotation of the stirring paddle 7, and the uniformity of a temperature field in the whole low-temperature tank is guaranteed. In this embodiment, a baffle 9 is provided between the paddles 7 and the support 3, with a space between the bottom of the baffle 9 and the bottom inside the tank housing 1. The motor 8 is started, the motor 8 drives the stirring paddle 7 to rotate, so that the low-temperature medium on the left side of the baffle 9 flows upwards and bypasses the top of the baffle 9, the low-temperature medium bypassing the top of the baffle 9 enters the right side of the baffle 9, and the low-temperature medium bypasses the bottom of the baffle 9 and enters the left side of the baffle 9, so that circular flow is formed.
Temperature control system includes temperature controller and temperature sensor, and temperature sensor gathers the temperature of the low temperature medium of splendid attire in groove shell 1 and feeds back the measured temperature to temperature controller, adjusts the output of cold source and heat source through temperature controller, and then adjusts the temperature of the low temperature medium of splendid attire in groove shell 1. The low-temperature tank can adopt alcohol as a low-temperature heat transfer medium and can also adopt other anti-freezing solutions.
The freezing device comprises a heat conducting rod 10 and a liquid containing cup 11, wherein the heat conducting rod 10 is a hollow copper rod and is subjected to vacuum pumping treatment. The liquid containing cup 11 is used for containing liquid nitrogen, the liquid containing cup 11 is composed of a three-layer structure, the innermost layer is made of stainless steel, the stainless steel is wrapped by heat insulation materials, and the outermost layer is made of plastic materials. The water triple point bottle 12 is vertically placed on the support 3, the liquid containing cup 11 is arranged above the support 3, the heat conducting rod 10 is vertically inserted into the thermometer well 13 of the water triple point bottle, and the top of the heat conducting rod 10 is welded with the stainless steel of the liquid containing cup 11.
A large-scale water triple point bottle ice sleeve freezing method comprises the following steps:
1) before the freezing process is started, the low-temperature tank is started, and the working temperature of the low-temperature tank is stabilized at 0 ℃.
2) The method comprises the steps of placing a water triple point bottle 12 on a support 3 in a low-temperature tank for precooling for 30min, then inserting a heat conducting rod 10 of a freezer into a water triple point bottle thermometer well 13, filling alcohol into the water triple point bottle thermometer well 13, injecting liquid nitrogen into a liquid containing cup 11 of the freezer, taking heat away through evaporation of the liquid nitrogen, taking out the freezer after freezing for 10min, and placing the freezer on a support sheet 2 on a tank shell 1.
3) Taking out the water triple point bottle 12, manually shaking, generating ice crystals in the water triple point bottle 12 to form crystal nuclei, and rotating the water triple point bottle 12 to uniformly distribute the crystal nuclei in the water triple point bottle 12.
4) The water three-phase point bottle 12 is placed on the support 3 in the low-temperature tank again, the water three-phase point bottle thermometer well 13 is filled with alcohol again, the heat conducting rod 10 of the freezer is placed in the water three-phase point bottle thermometer well 13, liquid nitrogen is kept filled in the liquid containing cup 11 of the freezer all the time in the freezing process, freezing is continued, the ice sleeve begins to form along the direction from the inner wall to the outer wall of the water three-phase point bottle thermometer well 13, after freezing is restricted for 2min, the water three-phase point bottle 12 is taken out, and the ice sleeve is rotated to prevent an ice bridge from being generated.
5) And (3) placing the water triple point bottle 12 on the bracket 3 in the low-temperature tank, placing the heat conducting rod 10 of the freezer into the thermometer well 13 of the water triple point bottle to continue freezing, and repeating the operation until the thickness of the frozen ice sleeve reaches the required thickness.
The device and the method for freezing the ice sleeve have the advantages of low requirement on operators, high efficiency, uniform thickness of the ice sleeve and long service time.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.

Claims (1)

1. A large-scale water triple point bottle ice sleeve freezing method is characterized in that a large-scale water triple point bottle ice sleeve freezing device is adopted in the method, and comprises a low-temperature tank and a freezer;
the low-temperature tank comprises a tank shell (1), a support sheet (2), a support (3), a refrigerating system, a heating system, a circulating system and a temperature control system;
the supporting sheet (2) is of a circular ring structure, and the supporting sheet (2) is fixedly arranged on the outer wall of the groove shell (1) and used for placing a freezer;
the bracket (3) is used for placing a water triple point bottle (12), and the bracket (3) is soaked in a low-temperature medium contained in the tank shell (1);
the refrigeration system is used for providing a cold source for the low-temperature tank and comprises a compressor (4) and an evaporator (5); the compressor (4) is arranged below the tank shell (1), the evaporator (5) is arranged in the tank shell (1), and the compressor (4) is connected with the evaporator (5) through a refrigerant circulating pipeline;
the heating system is used for providing a heat source for the low-temperature tank, and the heating system is a heating resistance wire (6) arranged in the tank shell (1);
the circulating system comprises a motor (8) and a stirring paddle (7), the stirring paddle (7) is immersed in a low-temperature medium contained in the tank shell (1), the stirring paddle (7) is driven by a power output shaft of the motor (8), the low-temperature medium circularly flows from bottom to top through the rotation of the stirring paddle (7), and the uniformity of a temperature field in the whole low-temperature tank is ensured;
the temperature control system comprises a temperature controller and a temperature sensor, the temperature sensor collects the temperature of the low-temperature medium contained in the tank shell (1) and feeds the measured temperature back to the temperature controller, the output power of the cold source and the heat source is adjusted through the temperature controller, and then the temperature of the low-temperature medium contained in the tank shell (1) is adjusted;
the freezing device comprises a heat conducting rod (10) and a liquid containing cup (11), wherein the heat conducting rod (10) is a hollow copper rod; the liquid containing cup (11) is used for containing liquid nitrogen, the liquid containing cup (11) is composed of a three-layer structure, the innermost layer is made of stainless steel, the stainless steel is wrapped by a heat insulation material, and the outermost layer is made of plastic; the liquid containing cup (11) is arranged above the bracket (3), the heat conducting rod (10) is vertically inserted into the thermometer well (13) of the water triple point bottle, and the top of the heat conducting rod (10) is welded with the stainless steel of the liquid containing cup (11);
a baffle (9) is arranged between the stirring paddle (7) and the bracket (3), and a gap is formed between the bottom of the baffle (9) and the bottom in the tank shell (1);
the method comprises the following steps:
1) before the freezing process is started, the low-temperature tank is started, and the working temperature of the low-temperature tank is stabilized at 0 ℃;
2) placing a water triple point bottle (12) on a bracket (3) in a low-temperature tank for precooling for 30min, then inserting a heat conducting rod (10) of a freezer into a water triple point bottle thermometer well (13), filling alcohol into the water triple point bottle thermometer well (13), injecting liquid nitrogen into a liquid containing cup (11) of the freezer, carrying away heat through evaporation of the liquid nitrogen, taking out the freezer after freezing for 10min, and placing the freezer on a support sheet (2) on a tank shell (1);
3) taking out the water triple point bottle (12), manually shaking the water triple point bottle (12), enabling ice crystals to appear in the water triple point bottle (12) to form crystal nuclei, and rotating the water triple point bottle (12) to enable the crystal nuclei to be uniformly distributed in the water triple point bottle (12);
4) putting the water triple point bottle (12) on the support (3) in the low-temperature tank again, filling alcohol in the water triple point bottle thermometer well (13) again, putting the heat conducting rod (10) of the freezer into the water triple point bottle thermometer well (13), always keeping the liquid nitrogen in the liquid containing cup (11) of the freezer during the freezing process, continuing freezing, starting to form an ice sleeve along the inner wall of the water triple point bottle thermometer well (13) to the outer wall direction, taking out the water triple point bottle (12) after freezing is restricted for 2min, and rotating the ice sleeve to prevent the generation of an ice bridge;
5) and (3) placing the water triple point bottle (12) on a bracket (3) in a low-temperature groove, placing the heat conducting rod (10) of the freezer into a thermometer well (13) of the water triple point bottle to continue freezing, and repeating the operation until the thickness of the frozen ice sleeve reaches the required thickness.
CN201911071544.6A 2019-11-05 2019-11-05 Large-scale water triple-point bottle ice sleeve freezing device and method Active CN110736568B (en)

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CN113804331A (en) * 2021-09-15 2021-12-17 湖州唯立仪表科技有限公司 Multifunctional thermostatic bath with automatic reproduction of water-containing triple points and temperature control method
CN115165153B (en) * 2022-05-13 2024-04-16 山东省计量科学研究院 Automatic device for freezing water by liquid nitrogen and ice cover of three-phase point bottle and use method

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