CN217277999U - Organic chemical product crystallization point measuring device - Google Patents
Organic chemical product crystallization point measuring device Download PDFInfo
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- CN217277999U CN217277999U CN202220291544.8U CN202220291544U CN217277999U CN 217277999 U CN217277999 U CN 217277999U CN 202220291544 U CN202220291544 U CN 202220291544U CN 217277999 U CN217277999 U CN 217277999U
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Abstract
The utility model provides an organic chemical product crystallization point survey device, include: a water bath container having a water bath space therein; a crystallization sleeve assembly comprising a crystallization sleeve supported by a support frame and capable of being placed within the water bath space; a thermostatic bath having a thermostatic fluid capable of being introduced into the water bath space and forming a fluid circulation in the water bath space in line with the thermostatic bath. According to the utility model discloses, need not to adopt the water bath thermometer among the prior art can conveniently adjust the target temperature that heating bath or cooling bath, the water bath temperature can keep invariable in the sample test time span, need not to add at the upper portion in water bath space and covers the asbestos lid and can satisfy the constancy of temperature demand, and temperature control precision is high, can greatly improve the survey work efficiency of different organic chemical products crystallization points, and the commonality of device is higher.
Description
Technical Field
The utility model belongs to the technical field of carbon fiber production detects utensil design with raw materials, concretely relates to organic chemical products crystallization point survey device.
Background
At present, in the production process of polyacrylonitrile-based carbon fiber, one raw material used by polyacrylonitrile solution is dimethyl sulfoxide, the quality standard of the product generally implements GB/T21395, and the implementation standard of a detection method for the crystallization point of the dimethyl sulfoxide in the standard is GB/T7533: a method for measuring crystallization point of organic chemical products. The crystallization point measuring apparatus of this standard is mainly composed of a main thermometer, a water bath thermometer, a crystallization tube, a protection tube, a stopwatch, a stirrer, a heating bath, a cooling bath or dewar flask, an asbestos cover plate, and the like. Wherein the heating bath or cooling bath consists essentially of a 400mL or 500mL beaker. The heating or cooling principle of the heating bath, cooling bath or dewar is to adjust the temperature thereof by filling the medium for heating or cooling therein such as dry ice, liquid nitrogen, ice cubes or other reagents such as xylene, ethylene glycol, ethanol and the like, and it is necessary to adjust the amount of the cooling or heating substance or reagent and to measure and control the temperature of the water bath using a water bath thermometer in the adjustment process to achieve the target control temperature, and the water bath temperature adjustment and control process is cumbersome.
SUMMERY OF THE UTILITY MODEL
Therefore, the utility model provides an organic chemical products crystallization point survey device can overcome among the prior art organic chemical products crystallization point survey device water bath temperature need adopt the thermometer to measure the back and carry out artifical adjustment according to the condition, water bath temperature control and the loaded down with trivial details not enough of control process.
In order to solve the above problem, the utility model provides an organic chemical products crystallization point survey device, include:
a water bath container having a water bath space therein;
a crystallization sleeve assembly comprising a crystallization sleeve supported by a support frame and capable of being placed within the water bath space;
a thermostatic bath having a thermostatic fluid capable of being introduced into the water bath space and forming a fluid circulation in the water bath space in line with the thermostatic bath.
In some embodiments of the present invention, the substrate is,
the water bath container is provided with a jacket layer, and the jacket layer forms fluid circulation with the constant temperature groove and is communicated with the water bath space.
In some embodiments of the present invention, the substrate is,
the supporting frame comprises a cylindrical base body with an upward opening and a clamping assembly connected with the cylindrical base body into a whole, the water bath container is located in the cylindrical base body, and the clamping assembly clamps the crystallization sleeve.
In some embodiments of the present invention, the substrate is,
the clamping assembly comprises an upright rod, the bottom end of the upright rod is fixedly connected with the cylindrical base body, the top end of the upright rod is connected with a clamp holder, and the clamp holder is clamped on the outer wall of the crystallization sleeve; and/or the cylindrical seat body is made of transparent materials.
In some embodiments of the present invention, the substrate is,
the clamp holder comprises two clamping jaws which are oppositely arranged, clamping arc plates are arranged at opposite positions on the clamping jaws on two sides of the clamping jaws, and the clamp holder further comprises a clamping force adjusting part which can force the two clamping arc plates to approach.
In some embodiments of the present invention, the substrate is,
the clamping force adjusting part comprises a stud fixedly connected with one of the two clamping jaws, the free end of the stud penetrates to the outer side of the other of the two clamping jaws, and a dovetail nut is connected to the free end of the stud in a threaded mode.
In some embodiments of the present invention, the substrate is,
the clamping force adjustment member comprises a spring, the spring being between the two jaws.
In some embodiments of the present invention, the substrate is,
the clamping force adjusting component further comprises a guide post, the spring is sleeved on the guide post, and two ends of the guide post are slidably connected to the two clamping jaws.
In some embodiments of the present invention, the substrate is,
the pipe orifice plug of the crystallization sleeve is provided with a rubber plug with a hole, the rubber plug with the hole is provided with a part which is positioned outside the pipe orifice, and the diameter of the part is larger than the diameter of the pipe body of the crystallization sleeve.
In some embodiments of the present invention, the substrate is,
the upright stanchion is a telescopic pole.
The utility model provides a pair of organic chemical products crystallization point survey device need not to adopt the water bath thermometer among the prior art can conveniently adjust the heating bath or the target temperature that the cooling bathed, and the water bath temperature can keep invariable in the sample test time within range, need not to add the lid asbestos cover on the upper portion in water bath space and can satisfy the constancy of temperature demand, and the temperature control precision is high, can greatly improve the survey work efficiency of different organic chemical products crystallization points, and the commonality of device is higher.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus for determining a crystallization point of an organic chemical product according to an embodiment of the present invention (omitting a connecting pipeline between a thermostatic bath and a water bath container);
FIG. 2 is a schematic cross-sectional view taken along line A-A in FIG. 1;
fig. 3 is a partially enlarged view of fig. 2 at B.
The reference numerals are represented as:
1. a water bath container; 11. a jacket water inlet; 12. a jacket water outlet; 13. a jacket layer; 21. crystallizing the sleeve; 22. a rubber plug with a hole; 23. a thermometer; 24. a stirrer; 31. a cylindrical seat body; 32. erecting a rod; 33. a holder; 331. a clamping jaw; 332. clamping the arc plate; 333. a dovetail nut; 334. a spring; 335. a guide post; 336. a stud; 4. a thermostatic bath; 41. a water outlet; 42. a water return port.
Detailed Description
Referring to fig. 1 to 3, according to an embodiment of the present invention, there is provided an apparatus for measuring a crystallization point of an organic chemical product, the organic chemical product may be, for example, dimethyl sulfoxide, and may be other products according to different processes, the apparatus includes: a water bath container 1 having a water bath space therein; a crystallization sleeve assembly comprising a crystallization sleeve 21, the crystallization sleeve 21 being supported by a support frame and capable of being placed in the water bath space; the thermostatic bath 4 (for example, a low-temperature thermostatic bath specifically, and certainly, a high-temperature thermostatic bath, and the like may also be adopted under some working conditions), the thermostatic fluid (for example, thermostatic water specifically) that it has can be guided into the water bath space, and the water bath space and the thermostatic bath 4 form a fluid circulation in a straight line, the thermostatic bath 4 may be the thermostatic bath 4 that can meet the temperature adjustment requirement on the market.
Among this technical scheme, need not to adopt the water bath thermometer among the prior art can conveniently adjust the target temperature of heating bath (high low temperature constant temperature or high temperature constant temperature) or cooling bath (low temperature constant temperature), and the water bath temperature can keep invariable in the sample test time within range, need not to cover the asbestos lid in the upper portion in water bath space and can satisfy the constancy of temperature demand, and the temperature control precision is high, can greatly improve the survey work efficiency of different organic chemical products crystallization points, and the commonality of device is higher.
As is well known in the art, the crystallization sleeve 21 is comprised of a crystallization tube and a sleeve that are ground to match, with air filling between the crystallization tube and the sleeve, and in one particular embodiment, the crystallization tube has an inner diameter of about 25mm, a wall thickness of about 2mm, a length of about 120mm, a sleeve inner diameter of about 38mm, a wall thickness of about 2mm, and a length of about 150 mm.
The volume of the water bath container 1 is preferably 5000mL-6000mL, so as to ensure that the crystallization sleeve 21 has enough height to be deep below the water bath surface and the bottom is visible, and enough water is also used for keeping the water bath temperature constant.
In some embodiments, the water bath container 1 has the jacket layer 13, the jacket layer 13 forms a fluid circulation with the thermostatic bath 4 and is communicated with the water bath space, and the jacket layer 13 is specifically formed by the outer wall and the inner wall of the water bath container 1 at intervals, so that the water bath space of the water bath container 1 can be isolated from the external environment to a certain extent, and the temperature constancy of the fluid in the water bath space is further improved. As shown in fig. 1, the jacket layer 13 has a corresponding jacket water inlet 11 and a corresponding jacket water outlet 12, the thermostatic bath 4 has a corresponding water outlet 41 and a water return port 42, the water outlet 41 is communicated with the jacket water inlet 11 through a water inlet pipeline, the water return port 42 is communicated with the jacket water outlet 12 through a water return pipeline, and it can be understood that the thermostatic bath 4 is provided with a corresponding temperature adjusting module, a fluid circulation driving module, a temperature detecting module, and the like, so as to ensure the constant temperature circulation of the fluid, and in terms of specific selection of the thermostatic bath 4, the temperature control range thereof can be selected according to the crystallization point range of the liquid-solid sample (i.e., the organic chemical product), and further preferably, the temperature control precision of the thermostatic bath 4 is selected from digital display resolution of 0.001 ℃ and the temperature fluctuation degree of ± 0.005 ℃ ± 0.02 ℃.
Generally, the support frame is arranged independently from the water bath container 1, such a structure can achieve the purpose of supporting the crystallization sleeve 21, but the structure of the whole device is not compact enough, as a more preferable implementation manner, the support frame comprises a cylindrical base 31 with an upward opening and a clamping component connected with the cylindrical base 31 into a whole, the water bath container 1 is arranged in the cylindrical base 31, the clamping component clamps the crystallization sleeve 21, and at this time, the support frame can position and load the water bath container 1 on one hand, and can support and clamp the crystallization sleeve 21 on the other hand, so that the structure of the device is more compact and convenient to operate. Preferably, the cylindrical base 31 is made of a transparent material, such as a transparent PVC plate, so as to prevent the observation of the crystallization process in the crystallization sleeve 21 from being obstructed, and the height thereof can be set higher, so as to improve the stability of the whole apparatus.
In some embodiments, the clamping assembly includes an upright rod 32, a bottom end of the upright rod 32 is fixedly connected to the cylindrical base 31, a clamp 33 is connected to a top end of the upright rod 32, the clamp 33 is clamped on an outer wall of the crystallization sleeve 21, specifically, the clamp 33 includes two clamping jaws 331 disposed opposite to each other, clamping arc plates 332 are disposed at opposite positions on the clamping jaws 331 on two sides, the clamp 33 further includes a clamping force adjusting component, and the clamping force adjusting component can force the two clamping arc plates 332 to approach each other, that is, the clamping arc plates 332 can be opened and closed to some extent under the action of the clamping force adjusting component, so as to effectively clamp the crystallization sleeve 21. The opposite side of centre gripping arc 332 is equipped with the rubber pad to can increase with frictional force between the crystallization sleeve pipe 21 guarantees the reliability of centre gripping, can also form the buffering to too big clamping-force simultaneously, protects crystallization sleeve pipe 21's structure.
The upright rod 32 is a telescopic rod, so that the adaptability adjustment can be performed according to different capacities (different lengths) of the clamped crystallization sleeves 21, and the application range of the device is expanded.
In a specific embodiment, referring to fig. 2, the clamping force adjusting part comprises a stud 336 fixedly connected with one of the two clamping jaws 331, a free end of the stud 336 passes through the outer side of the other of the two clamping jaws 331, a dovetail nut 333 is screwed on the free end of the stud 336, and the clamping force of the clamping jaws 331 can be adjusted by screwing the dovetail nut 333.
In another specific embodiment, referring to fig. 3, the clamping force adjusting component comprises a spring 334, the spring 334 is located between the two clamping jaws 331, and it is understood that the spring 334 is set to be in a stretched state instead of a compression device, so as to ensure the reliable clamping of the clamping jaws 331 to the crystallization sleeve 21. Furthermore, the clamping force adjusting component further comprises a guide post 335, the spring 334 is sleeved on the guide post 335, and two ends of the guide post 335 are slidably connected to the two clamping jaws 331, so that the relative stability of the positions of the two clamping jaws 331 in the clamping process can be ensured.
As is well known in the art, the orifice plug of the crystallization cannula 21 is provided with the perforated rubber plug 22, on which the thermometer 23 is positioned, and the stirrer 24 is inserted, and the stirrer 24 can stir the sample in the crystallization cannula 21, unlike the prior art, the perforated rubber plug 22 has a portion outside the orifice and having a diameter larger than the diameter of the tube body of the crystallization cannula 21, and it can be understood that the whole circle diameter formed by the two holding arc plates 332 after holding the crystallization cannula 21 is equal to the diameter of the tube body, so that the dropping-off of the crystallization cannula 21 can be effectively prevented by the perforated rubber plug 22 having a large diameter.
The technical scheme of the utility model is further explained by combining a specific operation process as follows:
connecting a jacket beaker (namely the water bath container 1, the same below, with the capacity of 5000mL) with a low-temperature thermostatic bath (namely the thermostatic bath 4, the same below), and setting the temperature of the low-temperature thermostatic bath to be 13-15 ℃;
placing the crystallization tube in a sleeve (the crystallization tube and the sleeve are assembled together to form the crystallization sleeve 21) according to the method, clamping the crystallization sleeve 21 onto the clamping arc plate 332 of the clamping device 33, and fixing the crystallization sleeve in a water bath;
loading a liquid dimethyl sulfoxide sample into a crystallization tube of the crystallization sleeve 21, wherein the height of the sample is about (60 +/-1) mm, and the sample is adjusted to be completely submerged in a water bath;
plugging a rubber stopper 22 with a hole, into which a thermometer 23 and a stirrer 24 have been inserted, to the opening of the crystallization thimble 21, wherein the thermometer is a glass-like mercury thermometer having a division value of 0.1 ℃ in the range of 0 to 50 ℃ and a distance from a mercury bulb of the thermometer to the bottom of the tube of about (15 +/-1) mm;
and pulling the stirrer 24 up and down to start stirring the sample, observing the temperature of the sample and the temperature of the sample, stopping stirring when the sample is crystallized, suddenly raising the temperature of the sample at the moment, and reading the highest temperature of the rise to be the crystallization point of the sample.
It is readily understood by a person skilled in the art that the advantageous ways described above can be freely combined, superimposed without conflict.
The above description is only exemplary of the present invention and should not be construed as limiting the present invention, and any modifications, equivalents and improvements made within the spirit and principles of the present invention are intended to be included within the scope of the present invention. The above is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. An organic chemical product crystallization point survey device which characterized in that includes:
a water bath container (1) having a water bath space therein;
a crystallization sleeve assembly comprising a crystallization sleeve (21), the crystallization sleeve (21) being supported by a support frame and capable of being placed in the water bath space;
a thermostatic bath (4) having a thermostatic fluid that can be introduced into the water bath space and forms a fluid circulation in the water bath space in line with the thermostatic bath (4).
2. The apparatus for determining a crystallization point of an organic chemical product according to claim 1,
the water bath container (1) is provided with a jacket layer (13), and the jacket layer (13) forms fluid circulation with the constant temperature groove (4) and is communicated with the water bath space.
3. The apparatus for determining a crystallization point of an organic chemical product according to claim 1,
the supporting frame comprises a cylindrical base body (31) with an upward opening and a clamping assembly connected with the cylindrical base body (31) into a whole, the water bath container (1) is located in the cylindrical base body (31), and the clamping assembly clamps the crystallization sleeve (21).
4. The apparatus for determining crystallization point of organic chemical product according to claim 3,
the clamping assembly comprises an upright rod (32), the bottom end of the upright rod (32) is fixedly connected with the cylindrical base body (31), the top end of the upright rod (32) is connected with a clamp holder (33), and the clamp holder (33) is clamped on the outer wall of the crystallization sleeve (21); and/or the cylindrical seat body (31) is made of transparent materials.
5. The apparatus for determining crystallization point of organic chemical product according to claim 4,
the clamp holder (33) comprises two oppositely arranged clamping jaws (331), clamping arc plates (332) are arranged at opposite positions on the clamping jaws (331) on two sides, and the clamp holder (33) further comprises a clamping force adjusting component which can force the two clamping arc plates (332) to approach.
6. The apparatus for determining crystallization point of organic chemical product according to claim 5,
the clamping force adjusting part comprises a stud (336) fixedly connected with one of the two clamping jaws (331), the free end of the stud (336) passes to the outer side of the other of the two clamping jaws (331), and a dovetail nut (333) is in threaded connection with the free end of the stud (336).
7. The apparatus for determining a crystallization point of an organic chemical product according to claim 5,
the clamping force adjusting component comprises a spring (334), and the spring (334) is arranged between the two clamping jaws (331).
8. The apparatus for determining a crystallization point of an organic chemical product according to claim 7,
the clamping force adjusting component further comprises a guide column (335), the spring (334) is sleeved on the guide column (335), and two ends of the guide column (335) are slidably connected to the two clamping jaws (331).
9. The apparatus for determining crystallization point of organic chemical product according to claim 4,
the mouth of the crystallization sleeve (21) is plugged with a rubber plug (22) with a hole, and the rubber plug (22) with the hole is provided with a part which is positioned outside the mouth and has a diameter larger than the diameter of the tube body of the crystallization sleeve (21).
10. The apparatus for determining crystallization point of organic chemical product according to claim 4,
the upright rod (32) is a telescopic rod.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220291544.8U CN217277999U (en) | 2022-02-08 | 2022-02-08 | Organic chemical product crystallization point measuring device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220291544.8U CN217277999U (en) | 2022-02-08 | 2022-02-08 | Organic chemical product crystallization point measuring device |
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| Publication Number | Publication Date |
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| CN217277999U true CN217277999U (en) | 2022-08-23 |
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| CN202220291544.8U Active CN217277999U (en) | 2022-02-08 | 2022-02-08 | Organic chemical product crystallization point measuring device |
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