CN202844621U - Single-stage recycle normal-pressure or decompression vapor-liquid equilibrium kettle - Google Patents

Single-stage recycle normal-pressure or decompression vapor-liquid equilibrium kettle Download PDF

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Publication number
CN202844621U
CN202844621U CN 201220324680 CN201220324680U CN202844621U CN 202844621 U CN202844621 U CN 202844621U CN 201220324680 CN201220324680 CN 201220324680 CN 201220324680 U CN201220324680 U CN 201220324680U CN 202844621 U CN202844621 U CN 202844621U
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China
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heating kettle
vapour phase
vapor
condensate liquid
under reduced
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Expired - Fee Related
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CN 201220324680
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Chinese (zh)
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顾正桂
孙昊
韩仲强
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Nanjing Normal University
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Nanjing Normal University
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Abstract

The utility model relates to a single-stage recycle normal-pressure or decompression vapor-liquid equilibrium kettle. A heating kettle is adopted; a vapor-phase lifting tube is arranged above the heating kettle; a coiled pipe type condensation reflux machine is connected above the vapor-phase lifting tube; a condensate reflux inlet of the coiled pipe type condensation reflux machine is connected with a vapor-phase condensate receiver through a vacuum hose; a spherical condenser pipe is connected above the vapor-phase condensate receiver; a reflux inlet of the vapor-phase condensate receiver is connected with the heating kettle through the vacuum hose; a water-bath thermal insulation tube is arranged on the outer part of the vapor-phase lifting tube; and temperature measuring ports are formed in the coiled pipe type condensation reflux machine and the heating kettle. According to the single-stage recycle normal-pressure or decompression vapor-liquid equilibrium kettle, the structure is simple, vapor-phase temperature can be constant easily, a vapor phase and a liquid phase do not have no temperature difference, stable normal-pressure or decompression vapor-liquid equilibrium can be achieved, the accurate measured result is accurate, and kettle is suitable for selecting solvents for extractive distillation and measuring normal-pressure or decompression vapor-liquid equilibrium data of a multi-component system.

Description

Single-stage circulation normal pressure or VLE under reduced pressure still
Technical field
The utility model relates to a kind of Vapor-Liquid Equilibrium Still, relates in particular to a kind of single-stage circulation normal pressure or VLE under reduced pressure still.
Background technology
Extraction and rectification separation method is widely used in the fields such as chemical industry, medicine, environmental protection, and can the extracting rectifying process realize, applicable effect how, and is except with extraction equipment is relevant, also relevant with extractant.The extractant system of selection is more, and the screening of extraction distillation solvent is method, empirical value method, data base querying by experiment, the methods such as computer aided molecular design (CAMD).Wherein experimental technique has direct method, chromatography, ebulliometer method, air lift method etc.That the screening that utilizes the Vapor-Liquid Equilibrium Still direct method to carry out extractant has is simple to operate, visual phenomenon, both can be qualitative also can be quantitative etc. advantage.But along with technology is constantly updated, the decompression extraction and rectification separation method occurred now, at this moment, then needed to carry out under reduced pressure by Vapor-Liquid Equilibrium Still the screening of extractant.
At present, all there is complex structure in the VLE under reduced pressure still of domestic existing employing, the problem such as is inconvenient to dismantle, and is not suitable for the laboratory and carries out simply and easily operation experiments.In the Vapor-Liquid Equilibrium Still that at present normal pressure adopts, Gillespie still and Rose still are simple in structure because of it, but and the VLE data under Accurate Determining constant voltage or the constant temperature, be considered to comparatively desirable a kind of.But, in case be used for depressurized system, then there are some problems, mainly contain following 4 points: vapour phase can't be preserved, and can directly be depressurized device and take away, can't reach VLE; Reach equilibration time longer, generally need about 4 hours; Required sample is more; When measuring the larger system of relative volatility, there is error to a certain degree.
Because the defective that above-mentioned existing single-stage circulation VLE under reduced pressure still exists, the design people, actively research and innovation in addition to founding a kind of single-stage circulation VLE under reduced pressure still of new structure, makes it have more practicality.
Summary of the invention
Above-mentioned deficiency for prior art, the purpose of this utility model is single-stage circulation normal pressure or the VLE under reduced pressure still of design new construction, success keep gas here, reach VLE, and guarantee up and down two the temperature-measuring port temperature difference<0.1 ℃, make full still temperature equalization, the concentration gradient elimination, dwindle the volume of heating kettle and vapour phase condensate liquid recipient, the boiling explosion phenomenon that exists in the decompression distillation is carried out safe alleviation, and increase magnetic stirring apparatus, purpose is to increase the liquid phase uniformity coefficient, shorten equilibration time, reduce required sample size.
The purpose of this utility model and solve its technical problem and realize by the following technical solutions.According to single-stage circulation normal pressure or the VLE under reduced pressure still that the utility model proposes, comprise heating kettle, the heating kettle top is provided with the vapour phase riser, vapour phase riser top is connected with the coiled condensation reflux device, the condensate liquid refluxing opening of coiled condensation reflux device connects vapour phase condensate liquid recipient by vacuum hose, the top of vapour phase condensate liquid recipient is connected with spherical condensation tube, the refluxing opening of vapour phase condensate liquid recipient takes back heating kettle by vacuum hose, simultaneously be provided with the water bath heat preservation pipe in vapour phase riser outside, all be provided with temperature-measuring port on coiled condensation reflux device and the heating kettle.
Be provided with coil heater in the aforementioned heating kettle.
The bottom of aforementioned heating kettle is provided with magnetic stirring apparatus, keep in the still liquid phase rapid mixing evenly, shorten equilibration time, reduce required sample size.
Aforementioned heating kettle is provided with sample tap, and sample tap is arranged on the heating kettle middle part, and sample tap adopts capillary to be processed into.
Aforementioned heating kettle is provided with vapour phase condensate liquid refluxing opening, and vapour phase condensate liquid refluxing opening position is in the middle and lower part of heating kettle.
Comprise serpentine condenser and riser in the aforementioned coiled condensation reflux device housing, riser stretches out from housing bottom, and the top is communicated with housing; Serpentine condenser is enclosed within outside the riser and the riser top is higher than serpentine condenser; Described lower housing portion is provided with the condensate liquid refluxing opening.
Condensate liquid in the aforementioned coiled condensation reflux device flow in the vapour phase condensate liquid recipient by vacuum hose.
Aforementioned vapour phase condensate liquid recipient bottom is provided with sample tap.
Connect drying tube on the aforesaid spherical condensation tube, the terminal water pump that connects of drying tube.
The volume of aforementioned heating kettle is 100mL, and the volume of vapour phase condensate liquid recipient is 10~12mL.
Between aforementioned heating kettle and the vapour phase riser, between vapour phase riser and the coiled condensation reflux device, all adopt ground to be connected between spherical condensation tube and the vapour phase condensate liquid recipient.
Further improvement in the technical proposal can have following prioritization scheme:
1. heating kettle and vapour phase riser interface are done a large diameter bumping cushion space, to avoid existing in the vapour phase riser a large amount of liquid that come up because of bumping, affect VLE;
2. the sample tap of vapour phase condensate liquid recipient is connected with a plurality of piston mouths with valve by translation interface, and the piston mouth is connected with the conical flask with atmospheric valve, like this by a plurality of conical flasks, takes to obtain different vapour phase condensate liquid samples constantly.
Above each prioritization scheme can use separately, also can adopt simultaneously.
By technique scheme, single-stage circulation normal pressure of the present utility model or VLE under reduced pressure still have following advantages at least: the utility model is simple in structure, vapor phase temperature is easy to constant, phase is substantially without temperature difference, can reach stable normal pressure or VLE under reduced pressure, measurement result is accurate, is applicable to selection and multicomponent system vapour-liquid normal pressure or the decompression equilibrium data measurement of extraction distillation solvent.Cancelled vapour liquid separator on traditional Vapor-Liquid Equilibrium Still and the liquid drain pipe of vapour liquid separator, success keep gas here, guaranteed the VLE under the reduced pressure, shortened the length of whole riser, and carried out water bath heat preservation, and adopted simultaneously up and down two temperature-measuring ports, can guarantee that the vapour-liquid temperature difference drops to minimum, make full still temperature equalization, the concentration gradient elimination increases magnetic stirring apparatus, guarantees the liquid phase uniformity coefficient, shorten equilibration time, reduce required sample size.Prioritization scheme arranges place bumping buffering and arranges on heating kettle top, avoid existing in the vapour phase riser a large amount of liquid that come up because of bumping, affects VLE; The sample tap of vapour phase condensate liquid recipient is connected with a plurality of piston mouths with valve by translation interface, and the piston mouth is connected with the conical flask with atmospheric valve, like this by a plurality of conical flasks, takes to obtain different vapour phase condensate liquid samples constantly.
In sum, the single-stage circulation normal pressure of the utility model special construction or VLE under reduced pressure still, it has above-mentioned many advantages and practical value, thereby more is suitable for practicality.
Above-mentioned explanation only is the general introduction of technical solutions of the utility model, for can clearer understanding technological means of the present utility model, and can be implemented according to the content of specification, below with preferred embodiment of the present utility model and cooperate accompanying drawing to be described in detail as follows.
Description of drawings
Fig. 1 is traditional Gillespie Vapor-Liquid Equilibrium Still structural representation.
Fig. 2 is the utility model single-stage circulation normal pressure or VLE under reduced pressure still structural representation.
Fig. 3 is the local structure for amplifying schematic diagram of coiled condensation reflux device.
The specific embodiment
Be to reach technological means and the effect that predetermined utility model purpose is taked for further setting forth the utility model, below in conjunction with accompanying drawing and preferred embodiment, the specific embodiment of the present utility model be described in detail as follows.
With reference to Fig. 2, single-stage circulation normal pressure or VLE under reduced pressure still, in heating kettle 9, be provided with coiled electric heater 7, heating kettle 9 outer surfaces are provided with coiled electric heater import 2 and coiled electric heater outlet 4, and heating kettle 9 is provided with liquid phase sample tap 3, charge door 5 and the first vapour phase condensate liquid refluxing opening 6; Heating kettle liquid phase sample tap 3 positions are at the still middle part, and liquid phase sample tap 3 adopts capillary to be processed into, and level control is in the middle and upper part of heating kettle 9 in the heating kettle 9, and the first vapour phase condensate liquid refluxing opening 6 is positioned at the middle and lower part of heating kettle 9, to reach the effect of fluid-tight; Also be provided with first on the heating kettle 9
Temperature-measuring port 1, heating kettle 9 tops carry out the part and amplify processing, to reach bumping are carried out buffered, are placed with magneton 8 in the heating kettle 9; Use magnetic stirrer, keep heating kettle 9 interior liquid phase rapid mixing even, shorten equilibration time, reduce required sample size; Heating kettle 9 tops are provided with vapour phase riser 13, are provided with the water bath heat preservation pipe in vapour phase riser 13 outsides, recirculated water adopts to advance down, on go out mode, be positioned at 9 two sides of equilibrium still, prevent from producing in the chuck dead angle, assurance vapour phase riser about in the of 13 without temperature difference.Vapour phase riser 13 is connected with coiled condensation reflux device 11, and condensate liquid cools off by condensate liquid import 12 and condensate outlet 10, and coiled condensation reflux device 11 is provided with the second temperature-measuring port 14, measures vapor phase temperature.Coiled condensation reflux device 11 comprises serpentine condenser 32 and riser 28 such as Fig. 3 in the housing 31; Riser 28 stretches out from housing 31 bottoms, and the top is communicated with housing 31; 31 distances that 2mm is all arranged of the tube wall of serpentine condenser 32 and riser 28 and housing; Serpentine condenser 32 is enclosed within outside the riser 28, and riser 28 tops are than serpentine condenser 32 height, and the lower end is provided with ground 27.Housing 31 bottoms are provided with the second vapour phase condensate liquid refluxing opening 15, exhaust outlet 34 and discharging opening 35, all are arranged on the outer wall of housing 31.The second vapour phase condensate liquid refluxing opening 15 that coiled condensation reflux device 11 arranges is connected with vapour phase condensate liquid recipient 24 by the first vacuum hose 20, the top of vapour phase condensate liquid recipient 24 is connected with spherical condensation tube 18, prevented that uncooled gas from being taken away by water pump, adopt spherical condensation tube condensate liquid import 21 and spherical condensation tube condensate outlet 19 to cool off, spherical condensation tube 18 tops connect the drying tube 17 that drier is housed, airborne moisture from entering system when preventing normal pressure, the end of drying tube 17 connects water pumps by the 3rd vacuum hose 16, controls the pressure of whole heating kettle 9 systems.Vapour phase condensate liquid in the vapour phase condensate liquid recipient 24 connects back the first vapour phase condensate liquid refluxing opening 6 on the heating kettle 9 through the 3rd refluxing opening 22 of vapour phase condensate liquid recipient by the second vacuum hose 23, the bottom of vapour phase condensate liquid recipient 24 is provided with condensate liquid sample tap 25, simultaneously, heating kettle 9, vapour phase riser 13, spherical condensation tube 18, coiled condensation reflux device 11 is connected with vapour phase condensate liquid recipient and is all adopted ground to connect, during use, the ground place need spread vaseline, also need wrap up unsintered tape in case of necessity.The first vapour phase condensate liquid refluxing opening 6, the second vapour phase condensate liquid refluxing opening 15, the 3rd refluxing opening 22 connect by the 3rd vacuum hose 16, the first vacuum hose 20, the second vacuum hose 23, are convenient to dismounting.Heating kettle 9 volumes are 100mL, and vapour phase condensate liquid recipient 24 volumes are 10mL.
The scope of application of single-stage circulation normal pressure of the present utility model or VLE under reduced pressure still is: adopt the pressure that connects water pump control equilibrium still system, can measure the vapor-liquid equilibrium data under normal pressure or the decompression different pressures condition; Adopt electrical heating, can measure the vapor-liquid equilibrium data under the high low temperature condition of different temperatures; Heating kettle 9 is less, the high or sample that is difficult to buy of particularly suitable price.When measuring the atmospheric steam liquid equilibrium data, can connect in spherical condensation tube 18 upper ends drying tube 17, in order to avoid airborne water vapour enters, affect vapour phase and form.
The operating procedure of the utility model single-stage circulation normal pressure or VLE under reduced pressure still is as follows:
(1) oven dry (or cleaning up) package unit;
(2) air-tightness of inspection package unit;
(3) charge door from heating kettle 9 adds raw material and extractant;
(4) the switch situation of detection valve connects water pump, the pressure of control package unit;
(5) start electric stirring, mixed liquor is fully mixed;
(6) open condensed water and recirculated water;
(7) open electrical heating, control heating kettle 9 temperature;
(8) vapour phase upper and lower temperature difference<0.1 ℃ waits to form constant, gets vapour phase condensate liquid and liquid phase and analyzes.
The above, it only is preferred embodiment of the present utility model, be not that the utility model is done any pro forma restriction, although the utility model discloses as above with preferred embodiment, yet be not to limit the utility model, any those skilled in the art, within not breaking away from the technical solutions of the utility model scope, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be the content that does not break away from technical solutions of the utility model, any simple modification that foundation technical spirit of the present utility model is done above embodiment, equivalent variations and modification all still belong in the scope of technical solutions of the utility model.

Claims (10)

1. a single-stage circulation normal pressure or VLE under reduced pressure still, comprise heating kettle, described heating kettle top is provided with the vapour phase riser, it is characterized in that: described vapour phase riser top is connected with the coiled condensation reflux device, the condensate liquid refluxing opening of described coiled condensation reflux device connects vapour phase condensate liquid recipient by vacuum hose, the top of described vapour phase condensate liquid recipient is connected with spherical condensation tube, the refluxing opening of described vapour phase condensate liquid recipient takes back described heating kettle by vacuum hose, simultaneously be provided with the water bath heat preservation pipe in described vapour phase riser outside, all be provided with temperature-measuring port on described coiled condensation reflux device and the described heating kettle.
2. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, be provided with coil heater in the described heating kettle.
3. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, the bottom of described heating kettle is provided with magnetic stirring apparatus.
4. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, described heating kettle is provided with sample tap, and described sample tap is arranged on described heating kettle middle part, and described sample tap adopts capillary to be processed into.
5. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, described heating kettle is provided with vapour phase condensate liquid refluxing opening, and described vapour phase condensate liquid refluxing opening position is the middle and lower part of described heating kettle.
6. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, comprise serpentine condenser and riser in the described coiled condensation reflux device housing, riser stretches out from housing bottom, and the top is communicated with housing; Serpentine condenser is enclosed within outside the riser and the riser top is higher than serpentine condenser; Described lower housing portion is provided with the condensate liquid refluxing opening.
7. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, described vapour phase condensate liquid recipient bottom is provided with sample tap.
8. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, connect drying tube on the described spherical condensation tube, the terminal water pump that connects of described drying tube.
9. according to single-stage circulation normal pressure claimed in claim 1 or VLE under reduced pressure still, it is characterized in that, the volume of described heating kettle is 100mL, and the volume of described vapour phase condensate liquid recipient is 10~12mL.
10. according to the described single-stage circulation normal pressure of the arbitrary claim of claim 1~9 or VLE under reduced pressure still, it is characterized in that, between described heating kettle and the described vapour phase riser, between described vapour phase riser and the described coiled condensation reflux device, all adopt ground to be connected between described spherical condensation tube and the described vapour phase condensate liquid recipient.
CN 201220324680 2012-07-06 2012-07-06 Single-stage recycle normal-pressure or decompression vapor-liquid equilibrium kettle Expired - Fee Related CN202844621U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106442897A (en) * 2016-11-26 2017-02-22 宁波工程学院 Decompression gas-liquid balance measuring system
CN107515281A (en) * 2017-10-03 2017-12-26 宁波工程学院 A kind of VLE under reduced pressure system with automatic pressure-controlled function
CN108508057A (en) * 2018-06-26 2018-09-07 常州大学 A kind of low pressure phase equilibrium experimental device and on-line period measurement method
CN108548837A (en) * 2018-06-26 2018-09-18 常州大学 A kind of measuring device of low-voltage high-temperature equilibrium
CN108627535A (en) * 2017-12-29 2018-10-09 泰州学院 Dynamic method vapour-liquid equilibrium measurement device

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106442897A (en) * 2016-11-26 2017-02-22 宁波工程学院 Decompression gas-liquid balance measuring system
CN106442897B (en) * 2016-11-26 2018-10-19 宁波工程学院 A kind of decompression vapor liquid equilibrium measurement system
CN107515281A (en) * 2017-10-03 2017-12-26 宁波工程学院 A kind of VLE under reduced pressure system with automatic pressure-controlled function
CN108627535A (en) * 2017-12-29 2018-10-09 泰州学院 Dynamic method vapour-liquid equilibrium measurement device
CN108508057A (en) * 2018-06-26 2018-09-07 常州大学 A kind of low pressure phase equilibrium experimental device and on-line period measurement method
CN108548837A (en) * 2018-06-26 2018-09-18 常州大学 A kind of measuring device of low-voltage high-temperature equilibrium
CN108548837B (en) * 2018-06-26 2020-11-24 常州大学 Low-pressure high-temperature phase equilibrium data measuring device
CN108508057B (en) * 2018-06-26 2023-07-25 常州大学 Low-voltage phase balance experimental device and online sampling and measuring method

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20130403

Termination date: 20150706

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