阅读说明：本技术 一种双氧弹绝热式热量计及燃烧热测量方法 (Dioxygen bomb heat insulation type calorimeter and combustion heat measuring method ) 是由 胡彪 谭中柱 何帅 刘云超 肖珍芳 罗建明 陈超 陈岳飞 于 2021-08-16 设计创作，主要内容包括：本发明公开了一种双氧弹绝热式热量计及燃烧热测量方法,一种双氧弹绝热式热量计包括外筒系统,包括外筒以及第一氧弹,所述外筒内用于填充第一水层,所述第一氧弹置于所述第一水层内；所述外筒由隔热材质制成；内筒系统,包括内筒以及第二氧弹,所述内筒设于外筒内；所述内筒内用于填充第二水层,所述第二氧弹置于所述第二水层内；所述内筒由隔热材质制成。一种燃烧热测量方法,采用所述的双氧弹绝热式热量计进行燃烧热测量；包括,步骤一；步骤二；步骤三；步骤四；步骤五。本发明通过双氧弹的结构解决内外筒之间的热交换,测试过程中可避免了量热系统与外界的热交换,提高测量准确度。(The invention discloses a dioxygen bomb heat insulation type calorimeter and a combustion heat measuring method, wherein the dioxygen bomb heat insulation type calorimeter comprises an outer cylinder system, an outer cylinder system and a first oxygen bomb, wherein a first water layer is filled in the outer cylinder system, and the first oxygen bomb is arranged in the first water layer; the outer cylinder is made of heat insulation materials; the inner cylinder system comprises an inner cylinder and a second oxygen bomb, and the inner cylinder is arranged in the outer cylinder; the inner barrel is used for filling a second water layer, and the second oxygen bomb is arranged in the second water layer; the inner cylinder is made of heat insulation materials. A combustion heat measuring method adopts the dioxygen bomb heat insulation type calorimeter to measure combustion heat; comprises the steps of; step two; step three; step four; and step five. The invention solves the heat exchange between the inner cylinder and the outer cylinder through the structure of the dioxygen bomb, can avoid the heat exchange between a calorimetric system and the outside in the test process, and improves the measurement accuracy.)

1. A thermal insulation type calorimeter with a dioxygen bomb is characterized by comprising,

the outer cylinder system comprises an outer cylinder and a first oxygen bomb, wherein the outer cylinder is filled with a first water layer, and the first oxygen bomb is arranged in the first water layer; the outer cylinder is made of heat insulation materials;

the inner cylinder system comprises an inner cylinder and a second oxygen bomb, and the inner cylinder is arranged in the outer cylinder; the inner barrel is used for filling a second water layer, and the second oxygen bomb is arranged in the second water layer; the inner cylinder is made of heat insulation materials.

2. The thermoinsulating dioxygen bomb calorimeter of claim 1, wherein the external cartridge system further comprises a first temperature sensor for detecting the temperature of the first layer of water.

3. The thermoinsulating dioxygen bomb calorimeter of claim 2, wherein the inner barrel system further comprises a second temperature sensor for sensing the temperature of the second layer of water.

4. The thermoinsulating dioxygen bomb calorimeter of claim 1, wherein a first opening is formed in the top end of the outer cylinder, a first cover plate is hermetically sealed at the first opening, and the first cover plate is made of a heat insulating material.

5. The thermoinsulating dioxygen bomb calorimeter of claim 4, wherein a second opening is formed in the top end of the inner cylinder, a second cover plate is hermetically sealed at the second opening, and the second cover plate is made of a heat insulating material.

6. The thermoinsulating dioxygen bomb calorimeter of claim 5, wherein the first cover plate is flush and in sealed engagement with the second cover plate.

7. A thermal adiabatic calorimeter as set forth in claim 1, wherein a first stirrer is provided in the outer vessel, the first stirrer being for stirring the first water layer.

8. A thermal adiabatic calorimeter as set forth in claim 7, wherein a second stirrer is provided in the inner cylinder, the second stirrer being for stirring the second aqueous layer.

9. The dioxygen bomb heat-insulating calorimeter of claim 1, wherein the outer and inner cylinders are each coated with an insulating layer on their outer surface.

10. A combustion heat measuring method characterized by performing combustion heat measurement using the dioxygen bomb adiabatic calorimeter as set forth in any one of claims 1 to 9; comprises the steps of (a) preparing a mixture of a plurality of raw materials,

step one, adding distilled water into an inner cylinder;

step two, weighing benzoic acid in a second oxygen bomb crucible of the inner cylinder, loading the benzoic acid into a second oxygen bomb, binding an ignition wire, filling oxygen into the second oxygen bomb, closing a cover of the second oxygen bomb, and stabilizing for a period of time;

step three, adding distilled water into the outer cylinder;

step four, according to the water quantity ratio of the second water layer and the first water layer in the inner cylinder and the outer cylinder, weighing benzoic acid with corresponding mass in a first oxygen bomb crucible of the outer cylinder, loading the benzoic acid into the first oxygen bomb, binding an ignition wire, filling oxygen into the first oxygen bomb, closing a cover of the first oxygen bomb, and stabilizing for a period of time;

and step five, starting the test and observing the temperature change in the test process.

Technical Field

The invention relates to combustion heat measuring equipment, in particular to a dioxygen bomb heat insulation type calorimeter and a combustion heat measuring method.

Background

An oxygen bomb calorimeter is an instrument for measuring the heat of combustion of a substance. The basic principle is as follows: a certain amount of combustion heat standard substance benzoic acid is combusted in an oxygen bomb of a calorimeter, and the released heat enables the whole calorimetric system (comprising an inner cylinder, water or other media in the inner cylinder, the oxygen bomb, a stirrer, a thermometer and the like) to be heated from an initial state temperature T_ARaising to the final temperature T_BThen, a certain amount of the substance to be measured is subjected to combustion measurement under the same conditions as described above. Because the used calorimeters are the same and the temperature change of the calorimetric system is consistent, the heat value of the measured substance can be obtained.

The oxygen bomb calorimeter can be divided into an isothermal oxygen bomb calorimeter (isothermal calorimeter for short) and an adiabatic oxygen bomb calorimeter (adiabatic calorimeter for short) according to the calorimetric principle. The outer cylinder of the constant temperature calorimeter has constant temperature, and the temperature difference exists between the inner cylinder and the outer cylinder, so that the inner cylinder and the outer cylinder have heat exchange and need to be cooled and corrected. The constant-temperature calorimeter is relatively complex in operation steps and calculation, but the instrument is simple in structure and easy to maintain.

The outer cylinder temperature of the heat insulation type calorimeter can automatically track the inner cylinder temperature and is always consistent with the inner cylinder temperature, and the temperature difference does not exist between the inner cylinder and the outer cylinder, so that heat exchange does not exist, and cooling correction is not needed. Therefore, the adiabatic calorimeter is simple to operate and calculate, but the instrument is complex in structure and difficult to maintain. The heat insulation type calorimeter can be divided into an electric heating heat insulation calorimeter and a vacuum heat insulation calorimeter. The electric heating heat insulation calorimeter enables the temperature of the outer cylinder to follow the temperature of the inner cylinder through electric heating when the temperature of the inner cylinder changes. The vacuum heat insulation calorimeter has the advantages that the outer cylinder is vacuum, the vacuum has good blocking effect on two heat transfer modes of heat conduction and convection, and heat exchange is blocked well.

At present, most of domestic manufacturers produce isothermal calorimeters, and only a few foreign manufacturers produce adiabatic calorimeters. In the test process of the isothermal calorimeter, heat transfer can be generated between the inner cylinder and the outer cylinder, and although corresponding compensation amount is adopted in the heat calculation process, the calculation is difficult to be accurate, and the phenomenon of inaccurate isothermal is easily caused. Meanwhile, when the temperature of the outer barrel of the electric heating heat insulation calorimeter changes along with the temperature of the inner barrel, the temperature of the outer barrel is difficult to accurately follow the temperature of the inner barrel due to heating inertia. The upper cover of the vacuum heat insulation calorimeter is not vacuum, when the temperature of the inner cylinder rises, the vacuum leakage of the outer cylinder is easily caused, and meanwhile, the experimental process of the vacuum heat insulation calorimeter is long in period, and the end of the period cannot be judged.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention provides a thermal insulation type calorimeter with a dioxygen bomb, which solves the problem of heat exchange between an inner cylinder and an outer cylinder through the structure of the dioxygen bomb so as to realize system thermal insulation.

The second objective of the present invention is to provide a combustion heat measuring method, which can avoid the heat exchange between the calorimetric system and the outside during the testing process, and improve the measuring accuracy.

One of the purposes of the invention is realized by adopting the following technical scheme:

a thermal insulation type calorimeter with a dioxygen bomb comprises,

the outer cylinder system comprises an outer cylinder and a first oxygen bomb, wherein the outer cylinder is filled with a first water layer, and the first oxygen bomb is arranged in the first water layer; the outer cylinder is made of heat insulation materials;

the inner cylinder system comprises an inner cylinder and a second oxygen bomb, and the inner cylinder is arranged in the outer cylinder; the inner barrel is used for filling a second water layer, and the second oxygen bomb is arranged in the second water layer; the inner cylinder is made of heat insulation materials.

Further, the urceolus system still includes first temperature sensor, first temperature sensor is used for detecting the temperature of first water layer.

Further, the inner cylinder system further comprises a second temperature sensor, and the second temperature sensor is used for detecting the temperature of the second water layer.

Further, the top of urceolus is equipped with first opening, the sealed closing cap of first opening part has first apron, first apron is made by thermal-insulated material.

Furthermore, a second opening is formed in the top end of the inner barrel, a second cover plate is hermetically covered at the second opening, and the second cover plate is made of heat insulation materials.

Further, the first cover plate and the second cover plate are flush and in sealing engagement.

Further, a first stirrer is arranged in the outer barrel and used for stirring the first water layer.

Further, a second stirrer is arranged in the inner barrel and used for stirring the second water layer.

Further, the outer surfaces of the outer barrel and the inner barrel are wrapped with heat insulation layers.

The second purpose of the invention is realized by adopting the following technical scheme:

a combustion heat measuring method adopts the dioxygen bomb heat insulation type calorimeter to measure combustion heat; comprises the steps of (a) preparing a mixture of a plurality of raw materials,

step one, adding distilled water into an inner cylinder;

step two, weighing benzoic acid in a second oxygen bomb crucible of the inner cylinder, loading the benzoic acid into a second oxygen bomb, binding an ignition wire, filling oxygen into the second oxygen bomb, closing a cover of the second oxygen bomb, and stabilizing for a period of time;

step three, adding distilled water into the outer cylinder;

step four, according to the water quantity ratio of the second water layer and the first water layer in the inner cylinder and the outer cylinder, weighing benzoic acid with corresponding mass in a first oxygen bomb crucible of the outer cylinder, loading the benzoic acid into the first oxygen bomb, binding an ignition wire, filling oxygen into the first oxygen bomb, closing a cover of the first oxygen bomb, and stabilizing for a period of time;

and step five, starting the test and observing the temperature change in the test process.

Compared with the prior art, the invention has the beneficial effects that: a certain amount of substance to be measured and water are contained in the inner cylinder, the substance and the water are combusted in the inner cylinder oxygen bomb, the heat is transferred to a heat measuring system (the inner cylinder, the water, the oxygen bomb and the like) through the stirrer, and the whole heat measuring system absorbs the heat of all the substances to be combusted until the temperature of the heat measuring system is balanced. In order to prevent the occurrence of heat exchange between the inner cylinder and the outer cylinder, when the measured material of the inner cylinder is combusted, the calculated measured material placed in the oxygen bomb of the outer cylinder is synchronously combusted, so that the heat released by the synchronous combustion in the oxygen bomb of the inner cylinder and the oxygen bomb of the outer cylinder is respectively transferred to an inner cylinder system (the inner cylinder, water, the oxygen bomb and the like) and an outer cylinder system (the outer cylinder, the water, the oxygen bomb and the like) through the stirring rod, and the temperature of the two systems can be kept consistent in the heat transfer process by placing the water contained in the specific inner cylinder and the specific water and the measured material of the inner cylinder and the specific outer cylinder, thereby avoiding the heat exchange between the inner cylinder and the outer cylinder. At this time, the temperature detecting device detects the temperature change before and after the heat absorption of the thermal system in the inner cylinder and the outer cylinder, and directly calculates the heat capacity of the calorimeter or the heat productivity of the measured substance according to the change.

Drawings

FIG. 1 is a schematic structural diagram of the present invention.

In the figure: 10. an outer cylinder; 11. a first aqueous layer; 12. a first temperature sensor; 13. a first stirrer; 14. a first cover plate; 20. a first oxygen bomb; 30. an inner barrel; 31. a second aqueous layer; 32. a second temperature sensor; 33. a second agitator; 34. a second cover plate; 40. and a second oxygen bomb.

Detailed Description

The present invention is further described with reference to the accompanying drawings and specific embodiments, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict. Except as specifically noted, the materials and equipment used in this example are commercially available. Examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present application and are not to be construed as limiting the present application.

In the description of the present application, it is to be understood that the terms "upper", "lower", "front", "back", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present application and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present application. In the description of the present application, "a plurality" means two or more unless specifically stated otherwise.

In the description of the present application, it should be noted that unless otherwise specifically stated or limited, the terms "connected," "communicating," and "connected" are to be construed broadly, e.g., as meaning a fixed connection, a connection through an intervening medium, a connection between two elements, or an interaction between two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.

The terms "first," "second," and the like in the description and in the claims of the present application and in the above-described drawings are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.

The dioxygen bomb heat insulation type calorimeter shown in fig. 1 comprises an outer cylinder 10 system and an inner cylinder 30 system, wherein the outer cylinder 10 system comprises an outer cylinder 10 and a first oxygen bomb 20, the outer cylinder 10 can be filled with a first water layer 11, the first water layer 11 can be formed by distilled water filled in the outer cylinder 10, the first oxygen bomb 20 is placed in the first water layer 11, and the outer cylinder 10 is made of heat insulation materials.

The inner cylinder 30 system includes an inner cylinder 30 and a second oxygen bomb 40, the inner cylinder 30 is disposed in the outer cylinder 10, the inner cylinder 30 can be filled with a second water layer 31, similarly, the second water layer 31 can be formed by second distilled water filled in the inner cylinder 30, and the second oxygen bomb 40 is disposed in the second water layer 31; the inner cylinder 30 is made of a heat insulating material.

On the basis of the structure, by using the dioxygen heat insulation type heat timing device, a certain amount of measured substances and distilled water are contained in the inner cylinder 30 and are combusted in the oxygen bomb of the inner cylinder 30, the heat can be transferred to a heat measuring system (the inner cylinder 30, the second water layer 31, the second oxygen bomb 40 and the like), and the whole heat measuring system absorbs the heat of all the combusted substances until the temperature of the heat measuring system is balanced. In order to prevent the occurrence of heat exchange between the inner and outer cylinders 10, when the measured material in the inner cylinder 30 is combusted, the calculated measured material placed in the first oxygen bomb 20 in the outer cylinder 10 is combusted synchronously, so that the heat released by the synchronous combustion in the oxygen bomb of the inner and outer cylinder 10 is transferred to the inner cylinder 30 system (inner cylinder 30, second water layer 31, second oxygen bomb 40, etc.) and the outer cylinder 10 system (outer cylinder 10, first water layer 11, first oxygen bomb 20, etc.) respectively, and the temperature of the two systems can be kept consistent in the heat transfer process by placing the amount of the water and the measured material contained in the specific inner and outer cylinder 10, thereby avoiding the heat exchange between the inner and outer cylinders 10.

At this time, the temperature detection device detects a temperature change before and after the heat absorption of the thermal system in the inner cylinder 30 and the outer cylinder 10, and directly calculates the heat capacity of the calorimeter or the heat generation amount of the measured substance from the change.

Further, the tub 10 system further comprises a first temperature sensor 12, and the first temperature sensor 12 is used for detecting the temperature of the first water layer 11, so that when the temperature of the tub 10 system is detected, the temperature can be directly detected by the first temperature sensor 12, and the temperature detection is accurate and sensitive.

Similarly, the inner cylinder 30 system further includes a second temperature sensor 32, and the second temperature sensor 32 is used for detecting the temperature of the second water layer 31, that is, when detecting the temperature of the inner cylinder 30 system, the temperature can be directly detected by the second temperature sensor 32, and the temperature detection is accurate and sensitive.

In the detection, a detection control system may be provided for receiving the temperatures detected by the first temperature sensor 12 and the second temperature sensor 32, and performing recording analysis.

The first temperature sensor 12 and the second temperature sensor 32 may be implemented by other temperature detection devices such as a thermometer in the related art.

Further, the top end of the outer cylinder 10 is provided with a first opening, and the first opening can be used for taking and placing the combustion object in the first oxygen bomb 20 and replacing the first water layer 11 after one-time detection is completed. In addition, a first cover 14 is hermetically sealed at the first opening, and the first cover 14 is made of a heat insulation material, so that a sealed and heat insulation state is conveniently formed in the outer tub 10.

Similarly, the top end of the inner cylinder 30 is provided with a second opening, and the second opening can be used for taking and placing the comburent in the second oxygen bomb 40 and replacing the second water layer 31 after one-time detection is completed. In addition, a second cover plate 34 is hermetically covered at the second opening, and the second cover plate 34 is made of a heat insulation material, so that a sealed heat insulation state is conveniently formed in the inner cylinder 30.

Furthermore, the first cover plate 14 is flush with and in sealing engagement with the second cover plate 34, so that a sealing dead angle caused by the fact that the first cover plate 14 and the second cover plate 34 are stepped is prevented, and the sealing effect is better.

Further, the first stirrer 13 is provided in the outer tub 10, the first stirrer 13 is used for stirring the first water layer 11, and when the combustion heat test of the outer tub 10 is performed, the first stirrer 13 stirs the first water layer 11, so that the combustion heat in the first oxygen bomb 20 can be sufficiently transferred.

Similarly, a second stirrer 33 is provided in the inner cylinder 30, and the second stirrer 33 is used for stirring the second water layer 31. When the combustion heat test of the inner cylinder 30 is performed, the second stirrer 33 stirs the second water layer 31, so that the combustion heat in the second oxygen bomb 40 can be sufficiently transferred.

Further, the outer surfaces of the outer cylinder 10 and the inner cylinder 30 are wrapped with heat insulation layers, namely, the outer cylinder 10 has a better heat insulation effect with the external environment, and the inner cylinder 30 has a better heat insulation effect with the outer cylinder 10, so that a better heat insulation state is formed.

In this embodiment, stainless steel vacuum cup is selected for use to inner tube 30, and through the isolated heat exchange between inner tube 30 and the external environment of vacuum layer, the adiabatic state is really realized, guarantees the precision of test data. The inner cylinder 30 does not destroy the vacuum environment as much as possible, the bottom of the inner cylinder 30 does not open a water gap, the second cover plate 34 of the inner cylinder 30 can be made of heat insulating materials or vacuum interlayers, and the openings of the second cover plate 34 and the inner cylinder 30 are sealed by sealing rings or rubber rings, so that the heat is prevented from losing from the inner cylinder 30.

The measured substance is combusted in the oxygen bomb, the heat of the measured substance is transferred to a heat measuring system (the inner cylinder 30, water, the oxygen bomb and the like) through the second stirrer 33, and the whole heat measuring system absorbs the heat of all the combusted substances until the temperature of the heat measuring system is balanced. The temperature probe detects the temperature change before and after the heat absorption of the calorimetric system, and directly calculates the heat capacity of the calorimeter or the heat productivity of the measured substance according to the change.

The embodiment also provides a combustion heat measuring method, which adopts the above-mentioned thermal insulation calorimeter with the double oxygen bomb to measure the combustion heat; comprises the steps of (a) preparing a mixture of a plurality of raw materials,

step one, adding distilled water into an inner cylinder to form the second water layer;

step two, weighing benzoic acid in a second oxygen bomb crucible of the inner cylinder, loading the benzoic acid into a second oxygen bomb, binding an ignition wire, filling oxygen into the second oxygen bomb, closing a cover of the second oxygen bomb, and stabilizing for a period of time, wherein the stabilization period can be specifically 15 seconds;

step three, adding distilled water into the outer cylinder;

step four, according to the water quantity ratio of the second water layer and the first water layer in the inner cylinder and the outer cylinder and the heat capacity ratio of the inner cylinder and the outer cylinder in comprehensive consideration, weighing benzoic acid with corresponding mass in a first oxygen bomb crucible of the outer cylinder, loading the benzoic acid into a first oxygen bomb, binding an ignition wire, filling oxygen into the first oxygen bomb, closing a cover of the first oxygen bomb, stabilizing for a period of time, and also stabilizing for 15 seconds;

in the fourth step, recording the ratio of the distilled water amount in the outer cylinder to the distilled water amount in the inner cylinder, comprehensively considering the ratio of the heat capacities of the calorimetric systems of the inner cylinder and the outer cylinder, weighing benzoic acid according to the ratio, enabling the ratio of the mass of the benzoic acid in the outer cylinder to the mass of the benzoic acid in the inner cylinder to be the same as the ratio of the distilled water amount in the outer cylinder to the distilled water amount in the inner cylinder, and then carrying out combustion operation.

And step five, starting the test and observing the temperature change in the test process.

Specifically, if the ignition fails, the test needs to be carried out again. If a next test is needed, the first oxygen bomb or the second oxygen bomb is deflated and then cleaned, and the next test is started after the first oxygen bomb or the second oxygen bomb is wiped dry.

In addition, if the heat capacity is calibrated, 5 times of heat capacity tests are needed to calculate the average heat capacity, and if the data is out of tolerance, a supplementary test is needed; the calorific value test needs 6 times of tests, and the calorific value repeatability and the indicating value error are calculated.

And recording a test result after the test is finished, and analyzing and judging data.

While only certain features and embodiments of the application have been illustrated and described, many modifications and changes may occur to those skilled in the art (e.g., variations in sizes, dimensions, structures, shapes and proportions of the various elements, mounting arrangements, use of materials, colors, orientations, etc.) without materially departing from the scope and spirit of the invention in the claims.

Finally, it should be noted that: the above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention should not be limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.