阅读说明：本技术 一种用于化工原料比热测定的量热计样品池 (Calorimeter sample pool for specific heat determination of chemical raw materials ) 是由 史全 闫慧敏 于 2020-05-07 设计创作，主要内容包括：本发明涉及量热学中量热装置,具体地说是一种用于化工原料比热测定的量热计样品池,包括样品池主体、金属垫片、样品池上盖及样品池套筒,样品池主体为圆锥型筒体结构,顶部设置法兰保证样品池的密闭性；金属垫片针对样品池大小有具体的尺寸和机械强度；样品池上盖为带排气口的法兰盖,排气口外接密封装置,样品池上盖与样品池通过柱栓密封；样品池套筒具有与样品池主体相匹配的圆锥形薄壁筒体,采用无感双绕法外缠加热丝,在样品池套筒底部焊接一半圆柱型筒体,用于放置温度计。本发明的样品池工作温度为室温-600K,工作压力为真空-10Mpa,样品池主体与加热—测温单元分离,换样及清洗方便。(The invention relates to a calorimetric medium-heat device, in particular to a calorimeter sample cell for specific heat determination of chemical raw materials, which comprises a sample cell main body, a metal gasket, a sample cell upper cover and a sample cell sleeve, wherein the sample cell main body is of a conical barrel structure, and a flange is arranged at the top of the sample cell main body to ensure the airtightness of the sample cell; the metal gasket has specific size and mechanical strength according to the size of the sample cell; the upper cover of the sample cell is a flange cover with an exhaust port, the exhaust port is externally connected with a sealing device, and the upper cover of the sample cell and the sample cell are sealed through a stud; the sample cell sleeve is provided with a conical thin-wall cylinder body matched with the sample cell main body, a heating wire is wound outside by adopting a non-inductive double-winding method, and a semi-cylindrical cylinder body is welded at the bottom of the sample cell sleeve and used for placing a thermometer. The working temperature of the sample cell is room temperature-600K, the working pressure is vacuum-10 Mpa, and the sample cell main body is separated from the heating-temperature measuring unit, so that the sample changing and the cleaning are convenient.)

1. A calorimeter sample cell for specific heat determination of chemical raw materials is characterized in that: the sample cell comprises a sample cell main body (1), a flange (2), a metal gasket (3), a sample cell upper cover (4) and a sample cell sleeve (8), wherein the sample cell main body (1) is of a cylindrical structure with a bottom and an opening at the upper end, the opening end is provided with the flange (2) used for ensuring the sample cell tightness, and a plurality of notches (7) are uniformly formed in the flange (2) along the circumferential direction; the sample cell upper cover (4) is a flange cover of the exhaust port (5), namely the sample cell upper cover (4) is of a disc-shaped structure, the exhaust port (5) is arranged on the sample cell upper cover (4), a plurality of studs (6) are uniformly arranged on the periphery of the exhaust port (5) along the circumferential direction, the number of the studs (6) is the same as that of the notches (7), the studs correspond to the notches (7) one by one, and the sample cell upper cover (4) is inserted into the corresponding notches (7) through the studs (6) to realize the sealing connection with the sample cell main body (1); the metal gasket (3) is arranged between the flange (2) and the upper cover (4) of the sample cell; sample cell sleeve (8) are including thin wall barrel (9), heater strip (10) and thermometer sleeve (11), and this thin wall barrel (9) cover is in sample cell main part (1) surface, the surface winding of thin wall barrel (9) has heater strip (10), the bottom rigid coupling of thin wall barrel (9) has thermometer sleeve (11) that are used for placing the thermometer.

2. A calorimeter cell for the determination of the specific heat of chemical raw materials, according to claim 1, wherein: the sample cell main body (1) is a conical cylinder with a wide upper part and a narrow lower part, the height of the sample cell main body (1) is 10-35 mm, the outer diameter of the upper end is 15-30 mm, the outer diameter of the bottom is 10-20 mm, and the thickness is 0.9-2 mm; the material of the sample cell main body (1) is titanium alloy.

3. A calorimeter cell for the determination of the specific heat of chemical raw materials, according to claim 1, wherein: the flange (2) is a concave flange, namely the flange (2) is annular, an annular gasket groove (12) is formed in the periphery of the inner diameter of the flange (2), and the metal gasket (3) is accommodated in the gasket groove (12); the external diameter of flange (2) is 30 ~ 50mm, thickness is 5 ~ 15mm, and notch (7) of equipartition are circular on this flange (2), and the internal diameter of notch (7) is 4 ~ 6 mm.

4. A calorimeter cell for the determination of the specific heat of chemical raw materials, according to claim 1, wherein: the metal gasket (3) is annular, and the thickness is 3-5 mm.

5. A calorimeter cell for the determination of the specific heat of chemical raw materials, according to claim 1, wherein: the upper cover (4) of the sample cell is disc-shaped, and the thickness of the upper cover is 5-15 mm; the outer diameter of the stud (6) is 4-6 mm, and the length of the stud is 15-40 mm; the exhaust port (5) is a hollow cylinder, the sample cell main body (1) is connected with the sample cell upper cover (4) in a sealing mode and then communicated with the interior of the sample cell main body (1), the wall thickness of the exhaust port (5) is 1-3 mm, and the outer diameter of the exhaust port is 5-15 mm.

6. A calorimeter sample cell for the specific heat determination of chemical raw materials, according to claim 5, wherein: the lower surface of sample cell upper cover (4) is equipped with circular shape arch (13), and the centre of this arch (13) is opened has the confession gas vent (5) and the inside through-hole that communicates of sample cell main part (1), arch (13) insert in the hole of flange (2) after sample cell main part (1) and sample cell upper cover (4) sealing connection.

7. A calorimeter cell for the determination of the specific heat of chemical raw materials, according to claim 1, wherein: the thin-wall sleeve (9) is conical, the height of the thin-wall sleeve is 10-35 mm, the outer diameter of the upper end of the thin-wall sleeve is 15-30 mm, the outer diameter of the bottom of the thin-wall sleeve is 10-20 mm, and the wall thickness of the thin-wall sleeve is 0.5-1 mm; the heating wire (10) is an enameled snap wire with the diameter of phi 0.15-0.2 mm.

8. A calorimeter cell for the determination of the specific heat of chemical raw materials, according to claim 1, wherein: the thermometer sleeve (11) is a semi-cylindrical barrel with openings at two ends, the length is 5-15 mm, the wall thickness is 0.5-1 mm, and the outer radius of the semi-circle is 1-5 mm.

Technical Field

The invention relates to a calorimetric device, in particular to a calorimeter sample pool for measuring specific heat of chemical raw materials.

Background

The occurrence of potential safety hazards and safety accidents is always accompanied in the chemical production process, and the sensitive parameters of the accidents are often unknown. Sensitive parameters for measuring chemical safety comprise the maximum reaction rate reaching time TMRad of the runaway reaction, adiabatic temperature rise delta Tad, technical maximum temperature MTT, maximum temperature MTSR which can be reached by the runaway system and the like, and the accident can be prevented only by mastering the limit value under the runaway condition. In chemical production, the specific heat is generally measured by a continuous heating dynamic method, and the specific heat measurement has larger error due to insufficient balance time. Due to errors of specific heat in calculation and measurement methods, certain errors are caused in correction of sensitive parameters.

The intermittent heating method with sufficient balance time is an adiabatic calorimetry method with accurate measurement, and a measurement sample is generally a pure substance or multiple components which do not react, so that a sample cell is mostly designed in a closed mode without an exhaust function. However, due to specific heat measurement of chemical reaction substances, gas may be generated in the measurement process, but the existing sample cell cannot collect or reasonably lead out of the reactor.

Therefore, the sample pool of the adiabatic heat measuring device suitable for chemical reaction materials is urgently needed to be developed so as to meet the urgent need of the specific heat research of the current chemical materials.

Disclosure of Invention

Aiming at the requirement of chemical reaction on a calorimetric device, the invention aims to provide a calorimeter sample pool for specific heat determination of chemical raw materials. The working temperature of the calorimeter sample pool is room temperature-600K, the working pressure is vacuum-10 Mpa, the separation of the calorimeter sample pool and the heating-temperature measuring unit is realized, the calorimeter sample pool has the characteristics of high disassembly and replacement efficiency and convenient cleaning, and the whole tightness of the calorimeter sample pool is good, so that the reaction gas can be led out for collection and further characterization and analysis.

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

the sample cell comprises a sample cell main body, a flange, a metal gasket, a sample cell upper cover and a sample cell sleeve, wherein the sample cell main body is of a cylindrical structure with a bottom and an opening at the upper end, the opening end is provided with the flange used for ensuring the sample cell tightness, and the flange is uniformly provided with a plurality of notches along the circumferential direction; the sample cell upper cover is a flange cover of an exhaust port, namely the sample cell upper cover is of a disc-shaped structure, the exhaust port is arranged on the sample cell upper cover, a plurality of studs are uniformly arranged on the periphery of the exhaust port along the circumferential direction, the number of the studs is the same as that of the notches, the studs correspond to the notches one by one, and the sample cell upper cover is inserted into the corresponding notches through the studs to realize the sealing connection with the sample cell main body; the metal gasket is arranged between the flange and the upper cover of the sample cell; the sample pool sleeve comprises a thin-wall barrel, a heating wire and a thermometer sleeve, the thin-wall barrel is sleeved on the outer surface of the sample pool main body, the heating wire is wound on the outer surface of the thin-wall barrel, and the thermometer sleeve used for placing a thermometer is fixedly connected to the bottom of the thin-wall barrel.

Wherein: the sample cell main body is a conical cylinder with a wide upper part and a narrow lower part, the height of the sample cell main body is 10-35 mm, the outer diameter of the upper end of the sample cell main body is 15-30 mm, the outer diameter of the bottom of the sample cell main body is 10-20 mm, and the thickness of the sample cell main body is 0.9-2 mm; the material of the sample cell main body is titanium alloy.

The flange is a concave flange, namely the flange is circular, a circular gasket groove is arranged on the periphery of the inner diameter of the flange, and the metal gasket is contained in the gasket groove; the external diameter of flange is 30 ~ 50mm, thickness is 5 ~ 15mm, and the notch of equipartition is circular on this flange, and the internal diameter of notch is 4 ~ 6 mm.

The metal gasket is in a ring shape, and the thickness of the metal gasket is 3-5 mm.

The upper cover of the sample cell is disc-shaped, and the thickness of the upper cover is 5-15 mm; the outer diameter of the stud is 4-6 mm, and the length of the stud is 15-40 mm; the gas vent is a hollow cylinder, the sample cell main body is connected with the sample cell upper cover in a sealing mode and then communicated with the interior of the sample cell main body, the wall thickness of the gas vent is 1-3 mm, and the outer diameter of the gas vent is 5-15 mm.

The lower surface of the sample cell upper cover is provided with a circular bulge, a through hole for communicating the exhaust port with the interior of the sample cell main body is formed in the middle of the bulge, and the bulge is inserted into an inner hole of the flange after the sample cell main body is hermetically connected with the sample cell upper cover.

The thin-wall sleeve is conical, the height of the thin-wall sleeve is 10-35 mm, the outer diameter of the upper end of the thin-wall sleeve is 15-30 mm, the outer diameter of the bottom of the thin-wall sleeve is 10-20 mm, and the wall thickness of the thin-wall sleeve is 0.5-1 mm; the heating wire is an enameled snap yarn with the diameter of phi 0.15-0.2 mm.

The thermometer sleeve is a semi-cylindrical barrel with openings at two ends, the length is 5-15 mm, the wall thickness is 0.5-1 mm, and the outer radius of the semi-circle is 1-5 mm.

The invention has the advantages and positive effects that:

1. the sample cell main body is separated from the heating-temperature measuring unit, so that the sample cell is convenient to disassemble and assemble and has higher efficiency when being cleaned or replaced; meanwhile, the damage to the heating wire and the temperature measuring element in the cleaning and replacing process can be avoided.

2. The sample cell main body and the sample cell upper cover are connected by the flange, so that the sample cell is ensured to have good tightness, and no gas is leaked in the reaction.

3. The upper cover of the sample cell is connected with the exhaust port, so that generated gas can be collected and further analyzed, and the research on the reaction process is facilitated.

4. The sample cell main body and the sample cell sleeve are of conical surface cylindrical structures, so that components can be better contacted through mutual extrusion acting force, and heat transfer is facilitated.

5. The sample cell can be normally used in the range of room temperature to 600K and vacuum to 10Mp, and is suitable for most reactions in chemical production.

Drawings

FIG. 1 is a schematic view of the overall structure of the present invention;

FIG. 2 is a schematic structural view of a sample cell body and a flange according to the present invention;

FIG. 3 is a schematic structural diagram of the upper cover of the sample cell of the present invention;

FIG. 4 is a schematic view of the structure of a sample cell sleeve according to the present invention;

wherein: 1 is the sample cell main part, 2 is the flange, 3 is the metal gasket, 4 is the sample cell upper cover, 5 is the gas vent, 6 is the cylindricality lock, 7 is the notch, 8 is the sample cell sleeve, 9 is the thin arm barrel, 10 is the heater strip, 11 is the thermometer sleeve, 12 is the gasket groove, and 13 is the arch.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings.

As shown in fig. 1 to 4, the sample cell comprises a sample cell main body 1, a flange 2, a metal gasket 3, a sample cell upper cover 4 and a sample cell sleeve 8, wherein the sample cell main body 1 is a cylindrical structure with a bottom and an opening at the upper end, the opening end is provided with the flange 2 for ensuring the sample cell tightness, and a plurality of notches 7 are uniformly formed in the flange 2 along the circumferential direction; sample cell upper cover 4 is the blind flange of gas vent 5, and sample cell upper cover 4 is the disc structure promptly, is equipped with gas vent 5 on this sample cell upper cover 4, and the periphery of gas vent 5 evenly is equipped with a plurality of studs 6 along circumference, and the quantity of stud 6 is the same with notch 7, and the one-to-one, and sample cell upper cover 4 realizes in inserting corresponding notch 7 through each stud 6 and is connected with the sealing of sample cell main part 1. The metal gasket 3 is arranged between the flange 2 and the sample cell upper cover 4. The sample cell sleeve 8 comprises a thin-wall cylinder 9, a heating wire 10 and a thermometer sleeve 11, the thin-wall cylinder 9 is sleeved on the outer surface of the sample cell main body 1, the heating wire 10 is wound on the outer surface of the thin-wall cylinder 9 by adopting an inductionless double-winding method, and the thermometer sleeve 11 for placing a thermometer is fixedly connected to the bottom of the thin-wall cylinder 9.

The sample cell main body 1 is a conical cylinder with a wide upper part and a narrow lower part, the height of the sample cell main body 1 is 10-35 mm, the outer diameter of the upper end is 15-30 mm, the outer diameter of the bottom is 10-20 mm, and the thickness is 0.9-2 mm; the material of the sample cell main body 1 is titanium alloy.

The flange 2 of the embodiment is a concave flange, that is, the flange 2 is circular, a circular gasket groove 12 is arranged at the periphery of the inner diameter of the flange 2, and the metal gasket 3 is accommodated in the gasket groove 12; the external diameter of flange 2 is 30 ~ 50mm, thickness is 5 ~ 15mm, and the notch 7 of equipartition is circular on this flange 2, and the internal diameter of notch 7 is 4 ~ 6mm, and the notch 7 of this embodiment is six.

The metal gasket 3 is annular, and the thickness of the metal gasket is 3-5 mm, so that the metal gasket is suitable for a concave flange sealing surface type; the metal gasket 3 of the present embodiment is made of stainless steel.

The upper cover 4 of the sample cell in the embodiment is disc-shaped, and the thickness is 5-15 mm; the outer diameter of the stud 6 is 4-6 mm, and the length is 15-40 mm; the gas vent 5 is hollow cylinder, external sealing device, and after sample cell main part 1 and 4 sealing connection of sample cell upper cover, gas vent 5 is linked together with the inside of sample cell main part 1, and the wall thickness of this gas vent 5 is 1 ~ 3mm, and the external diameter is 5 ~ 15 mm. In this embodiment, a circular protrusion 13 is disposed on the lower surface of the sample cell upper cover 4, a through hole for communicating the exhaust port 5 with the interior of the sample cell main body 1 is formed in the middle of the protrusion 13, and the protrusion 13 is inserted into the inner hole of the flange 2 after the sample cell main body 1 and the sample cell upper cover 4 are hermetically connected.

The thin-wall sleeve 9 is conical and matched with the sample cell main body 1, the height of the thin-wall sleeve is 10-35 mm, the outer diameter of the upper end of the thin-wall sleeve is 15-30 mm, the outer diameter of the bottom of the thin-wall sleeve is 10-20 mm, and the wall thickness of the thin-wall sleeve is 0.5-1 mm; the heating wire 10 is an enameled snap wire with the diameter of 0.15-0.2 mm.

The thermometer sleeve 11 of this embodiment is the both ends open-ended semicylindrical barrel, and length is 5 ~ 15mm, and the wall thickness is 0.5 ~ 1mm, and semicircle external radius is 1 ~ 5 mm.

The using method of the invention comprises the following steps:

the following procedure was used to load and unload samples to measure specific heat of a substance:

(1) the sample cell main body 1, the flange 2, the metal gasket 3 and the upper cover 4 are washed and dried by using absolute ethyl alcohol and deionized water in sequence;

(2) placing the sample cell main body 1, the flange 2, the metal gasket 3 and the sample cell upper cover 4 on a balance, weighing for three times, and taking an average value;

(3) putting a sample to be detected into the sample cell main body, and covering the sample cell upper cover 4 by padding a metal gasket 3;

(4) weighing the sample on the balance for three times again, and taking an average value, wherein the mass difference between the previous weighing and the next weighing is the mass of the sample to be measured;

(5) the upper cover 4 of the sample cell is sealed with the main body 1 of the sample cell by a stud 6;

(6) the sample cell is sleeved in the sample cell sleeve 8, and good contact is ensured;

(7) a sealing device at the upper end of the exhaust port 5 is connected;

(8) after connecting other wiring or plug wires of the heat measuring device, starting heat capacity testing;

(9) and after the experiment is finished, taking down the sample cell with the sample cell upper cover, and cleaning the sample cell main body, the flange and the sample cell upper cover by using absolute ethyl alcohol and deionized water.