CN107261554A - A kind of small-sized Liquid-liquid equilibrium kettle - Google Patents

A kind of small-sized Liquid-liquid equilibrium kettle Download PDF

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Publication number
CN107261554A
CN107261554A CN201710307336.6A CN201710307336A CN107261554A CN 107261554 A CN107261554 A CN 107261554A CN 201710307336 A CN201710307336 A CN 201710307336A CN 107261554 A CN107261554 A CN 107261554A
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CN
China
Prior art keywords
liquid
sample tap
jacketed
phase sample
vial
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Pending
Application number
CN201710307336.6A
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Chinese (zh)
Inventor
陈赟
王友长
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South China University of Technology SCUT
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South China University of Technology SCUT
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Application filed by South China University of Technology SCUT filed Critical South China University of Technology SCUT
Priority to CN201710307336.6A priority Critical patent/CN107261554A/en
Publication of CN107261554A publication Critical patent/CN107261554A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0446Juxtaposition of mixers-settlers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a kind of small-sized Liquid-liquid equilibrium kettle.The small-sized Liquid-liquid equilibrium kettle includes thermometer, extraction phase sample tap, raffinate phase sample tap, agitating device, time-controlling arrangement, the vial of jacketed and glass ground joint bottle stopper;The vial outer layer of the jacketed is provided with circulating water outlet and circulation water inlet;The glass port grinding bottle is connected with thermometer, extraction phase sample tap and raffinate phase sample tap beyond the Great Wall;The agitating device includes stirring magneton and magnetic stirring apparatus, and the stirring magneton is located at the bottom in the vial of jacketed, and the magnetic stirring apparatus and time-controlling arrangement are located at the bottom of the vial outer layer of jacketed.The small-sized Liquid-liquid equilibrium kettle can either be stirred or stratification with temperature control all the time;And can control and remind stirring and time of repose so that experiment has more high efficiency and accuracy;It can avoid interfering during sampling so that data are more accurate;Sustainable carry out many experiments, stability is good.

Description

A kind of small-sized Liquid-liquid equilibrium kettle
Technical field
The invention belongs to field of chemical engineering, and in particular to a kind of small-sized Liquid-liquid equilibrium kettle.
Background technology
Liquid-liquid equilibrium kettle is a kind of less Liquid-liquid equilibrium kettle of capacity, for determining Liquid-liquid equilibrium data.Changing Learn in industry, extraction, the technique of distillation process and equipment design are required for accurate Liquid-liquid equilibrium data, the offer of this data Exact Design is extracted or the process operation parameter and equipment size of rectifying are most important, is widely used in extracting and dephenolizing, purification Etc. various fields.Although many data can be estimated using simulation softward, obtaining accurate Liquid-liquid equilibrium data can return Return the key parameter for obtaining thermodynamical equilibrium equation so that process simulation is more accurate.With the exploitation of new technology, new extractant is not Disconnected discovery and the continuous extension of abstraction technique application field, also non-someone of many Liquid-liquid equilibrium data determine, and are required to pass through The mode of measuring is to obtain design parameter to meet the demand of engineering calculation.
Either scientific research institutions, research institution's research and development or student experimenting operation are single to extraction to strengthen for Liquid-liquid equilibrium kettle The many-side such as understanding of member is all in daily use.Liquid-liquid equilibrium data are determined, phasor, analysis temperature, concentration on extraction is drawn out Influence of energy etc., is required to lot of experimental data.Experimentation needs to control the minor variations of concentration in temperature, liquid phase all to lead Biphase equilibrium is caused to produce movement.Some equilibrium stills can cause lower floor's sample sampling contaminated through upper strata sample when may remove layer sample; Some equilibrium stills clamp lower floor's sample using interface export closed with flexible pipe again, have one section of dead angle in outlet section, stirring is not Uniformly, and the flexible pipe easy leakage of inserting needle sampling repeatedly.Some equilibrium stills can not set stirring and layering time of repose, it is impossible to and When sample so that particularly under conditions of the experiment of high temperature due to sample place evaporate too long influence liquid-liquid equilibrium result Etc..
The content of the invention
For solve prior art shortcoming and defect in place of, it is an object of the invention to provide one kind control when, temperature control stirring Rationally, accurately and conveniently small-sized Liquid-liquid equilibrium kettle is sampled.
During Liquid-liquid equilibrium use, glass port grinding bottle the extraction phase sample tap in face and raffinate phase sampling beyond the Great Wall will be exposed to Mouth is connected with sebific duct and sealed so that liquid-liquid diphase, which is enclosed in vial, to be ensured not leak.The vial of jacketed is placed in and stirred Mix to utilize on device and stir magneton stirring mixing, and open circulation water management Phase Equilibrium Temperature, then beforehand through time-controlling arrangement Mixing time and layering time of repose are set, generally stirring more than 2 hours stands more than 18 hours, closes after stirring and stand, Recirculated water temperature control all the time, then a plastics small hose is connected by syringe stretched respectively by extraction phase sample tap and raffinate phase sample tap Enter sampling, now read temperature reading.Extractant or extract are added after sampling, changes circulating water temperature, continues to stir Carry out next sample measure.
The object of the invention is achieved through the following technical solutions:
A kind of small-sized Liquid-liquid equilibrium kettle, including thermometer, extraction phase sample tap, raffinate phase sample tap, agitating device, when Between control device, the vial of jacketed and glass ground joint bottle stopper;The vial outer layer (i.e. chuck) of the jacketed is provided with and followed Ring water out and circulation water inlet;The glass port grinding bottle is connected with thermometer, extraction phase sample tap and raffinate phase sample tap beyond the Great Wall; The agitating device includes stirring magneton and magnetic stirring apparatus, and the stirring magneton is located at vial inner bag (the i.e. glass of jacketed Glass bottle) in bottom, the magnetic stirring apparatus and time-controlling arrangement are located at the bottom of the vial outer layer of jacketed.
The time-controlling arrangement can set stirring and layering time of repose so that sampling much sooner, can prevent spy It is not because sample places the influence liquid-liquid equilibrium result that evaporates too long under conditions of the experiment of high temperature.
The glass port grinding bottle is connected with two sample taps beyond the Great Wall, and extraction phase sample tap bottom can be at Liquid-liquid equilibrium interface With up to glass port grinding bottle plug lower end any position, the design of raffinate phase sample tap bottom below Liquid-liquid equilibrium two-phase interface but Higher than more than stirring magneton and avoiding being stirred magneton collision.During sampling extraction phase and extraction can be directed respectively into using plastics small hose Yu Xiang so that sampling is not interfere with each other.
The glass port grinding bottle is connected with thermometer, continuous observation temperature beyond the Great Wall, and accurately obtains temperature information in sampling.
The outer layer of the vial of the jacketed is provided with circulation water inlet and circulating water outlet, circulation of the recirculated water from lower end Water inlet enters, from the circulating water outlet outflow to upper end.Made in mixing using recirculated water temperature control and using magneton is stirred It must stir, stirring stops the agitation of stirring magneton and temperature control stratification after terminating.
The inner bag distance from bottom raffinate phase sample tap bottom distance of the vial of the jacketed need to be more than cylindricality and stir magnetic 1.5 times of sub- diameter, to avoid causing impact damage to raffinate phase sample tap bottom during stirring magneton stirring.
The extraction phase sample tap bottom both can be more than two liquid phases, can also be in the extraction phase of upper strata.Can during sampling Plastics small hose is stretched into upper strata extraction phase and obtains the uniform fluid sample of typical hybrid.
The raffinate phase sample tap bottom is necessarily in lower floor's raffinate phase, but higher than stirring magneton.It will can be moulded during sampling Material small hose stretches into lower floor's raffinate phase and obtains the uniform fluid sample of typical hybrid.
A kind of described small-sized Liquid-liquid equilibrium kettle, although temperature can produce fluctuation in Liquid-liquid equilibrium continuous mode, But finally it is defined by sampling chronothermometer reading.
Compared with prior art, the present invention has advantages below and beneficial effect:
(1) can be closed by two sample taps with a conduit, it is to avoid two-phase is lost.
(2) can either it be stirred or stratification with temperature control all the time.
(3) it can control and remind stirring and time of repose so that experiment has more high efficiency and accuracy.
(4) it can avoid interfering when sampling so that data are more accurate.
(5) sustainable carry out many experiments, stability is good.
Brief description of the drawings
Fig. 1 is Liquid-liquid equilibrium kettle structural representation of the present invention, in figure:1- extraction phase sample taps, 2- thermometers, 3- raffinates Phase sample tap, 4- circulating water outlets, 5- extraction phases, 6- raffinate phases, 7- stirring magnetons, 8- time-controlling arrangements, 9- magnetic agitations Device, 10- circulation water inlets, the vial of 11- jacketeds, 12- ground glass stoppers.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited In this.
As shown in figure 1, Liquid-liquid equilibrium kettle of the present invention includes:Extraction phase sample tap 1, thermometer 2, raffinate phase sample tap 3, Time-controlling arrangement 8, agitating device, the vial 11 and glass ground joint bottle stopper 12 of jacketed;The outer layer of vial 11 of jacketed Provided with circulating water outlet 4, circulation water inlet 10;Thermometer 2, extraction phase sample tap 1 and raffinate are connected with glass ground joint bottle stopper 12 Phase sample tap 3.The agitating device includes stirring magneton 7 and magnetic stirring apparatus 9, and the stirring magneton 7 is located at the glass of jacketed Bottom in glass 11 inner bags of bottle, the magnetic stirring apparatus 9 and time-controlling arrangement 8 are located at the bottom of the outer layer of vial 11 of jacketed Portion.
Two sample taps are connected with glass ground joint bottle stopper 12, the bottom of extraction phase sample tap 1 can be at Liquid-liquid equilibrium interface With the up to lower end any position of glass port grinding bottle plug 12, the design of the bottom of raffinate phase sample tap 3 Liquid-liquid equilibrium two-phase interface with It is lower but higher than stirring magneton more than 7 and avoid being stirred magneton 7 and collide.During sampling extraction can be directed respectively into using plastics small hose Phase 5 and raffinate phase 6 so that sampling is not interfere with each other.
The outer layer of the vial 11 of jacketed is provided with circulation water inlet 10 and circulating water outlet 4, and recirculated water is followed from lower end Ring water inlet 10 enters, and is flowed out from the circulating water outlet 4 to upper end.Recirculated water temperature control is used in mixing and is utilized and stirs magnetic Son 7 to stir, and stirring stops the agitation of stirring magneton and temperature control stratification after terminating.
The bottom distance of 11 inner bag distance from bottom raffinate phase sample tap of vial 3 of jacketed need to be more than the stirring magneton of cylindricality 1.5 times of 7 diameters, to cause impact damage to the bottom of raffinate phase sample tap 3 when avoiding stirring magneton 7 from stirring.
The bottom of extraction phase sample tap 1 both can be more than two liquid phases, can also be in upper strata extraction phase 5.Can be by during sampling Plastics small hose stretches into upper strata extraction phase 5 and obtains the uniform fluid sample of typical hybrid.
The bottom of raffinate phase sample tap 3 is necessarily in lower floor's raffinate phase 6, but higher than stirring magneton 7.Can be by plastics during sampling Small hose stretches into lower floor's raffinate phase 6 and obtains the uniform fluid sample of typical hybrid.
Embodiment 1
Concrete operations are carried out with reference to accompanying drawing to be described as follows:
(1) extractant and extract are imported in the vial 11 of jacketed, adds stirring magneton 7, glass port grinding bottle Plug 12 is closed with conduit connection by extraction phase sample tap 1 and raffinate phase sample tap 3 after clogging.Will circulation water inlet 10 and recirculated water Outlet 4 is connected with temperature control pond, keeps equilibrium still temperature stabilization.
(2) equilibrium still is placed on agitator, opens agitator, is mixed using the stirring of magneton 7 is stirred, and when stirring is set Between.
(3) agitator is closed in stirring after terminating, and continues temperature control, keeps recirculated water flowing.Stratification, and set layering quiet Put the time.
(4) sample tap connection sealing duct is opened, connecting the soft tubule insertion extraction phase of a plastics with precision syringe samples Mouth 1, stretches into the accurate pipette samples of extraction phase 5, and write down temperature;Then the soft tubule of a plastics is connected with another precision syringe to insert Enter raffinate phase sample tap 3, stretch into the accurate pipette samples of raffinate phase 6, and write down temperature.Repeated sampling three times is to analyze respectively.
(5) open glass ground joint bottle stopper 12 and supplement extractant or extract, glass ground joint bottle stopper 12 beyond the Great Wall and connects two Individual sample tap, adjusts circulating water temperature, opens agitating device, carries out next measuring.
The small-sized Liquid-liquid equilibrium kettle of the present invention, is used, process stabilization is easy to operate, economical and efficient by long-term experiment, Data are accurate, are a kind of no-pollution experiment devices for being especially suitable for modernizing teaching and scientific research.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (3)

1. a kind of small-sized Liquid-liquid equilibrium kettle, it is characterised in that including thermometer, extraction phase sample tap, raffinate phase sample tap, stir Mix device, time-controlling arrangement, the vial of jacketed and glass ground joint bottle stopper;The vial outer layer of the jacketed is provided with and followed Ring water out and circulation water inlet;The glass port grinding bottle is connected with thermometer, extraction phase sample tap and raffinate phase sample tap beyond the Great Wall; The agitating device includes stirring magneton and magnetic stirring apparatus, and the stirring magneton is located at the bottom in the vial inner bag of jacketed Portion, the magnetic stirring apparatus and time-controlling arrangement are located at the bottom of the vial outer layer of jacketed.
2. a kind of small-sized Liquid-liquid equilibrium kettle according to claim 1, it is characterised in that the vial of the jacketed Inner bag distance from bottom raffinate phase sample tap bottom distance is more than 1.5 times of stirring magneton diameter.
3. a kind of small-sized Liquid-liquid equilibrium kettle according to claim 1, it is characterised in that the extraction phase sample tap bottom More than two liquid phases or in the extraction phase of upper strata;The raffinate phase sample tap bottom is in lower floor's raffinate phase, higher than stirring magnetic Son.
CN201710307336.6A 2017-05-04 2017-05-04 A kind of small-sized Liquid-liquid equilibrium kettle Pending CN107261554A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710307336.6A CN107261554A (en) 2017-05-04 2017-05-04 A kind of small-sized Liquid-liquid equilibrium kettle

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710307336.6A CN107261554A (en) 2017-05-04 2017-05-04 A kind of small-sized Liquid-liquid equilibrium kettle

Publications (1)

Publication Number Publication Date
CN107261554A true CN107261554A (en) 2017-10-20

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201195060Y (en) * 2008-04-29 2009-02-18 上海化工研究院 Atmosphere-pressure liquid-liquid equilibrium kettle
CN202724745U (en) * 2012-08-20 2013-02-13 南京师范大学 Jacket-type normal-pressure liquid-liquid balance kettle
CN205699576U (en) * 2016-04-19 2016-11-23 河南科技学院 A kind of novel liquid-liquid equilibrium still

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201195060Y (en) * 2008-04-29 2009-02-18 上海化工研究院 Atmosphere-pressure liquid-liquid equilibrium kettle
CN202724745U (en) * 2012-08-20 2013-02-13 南京师范大学 Jacket-type normal-pressure liquid-liquid balance kettle
CN205699576U (en) * 2016-04-19 2016-11-23 河南科技学院 A kind of novel liquid-liquid equilibrium still

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
郑铁生: "《临床生物化学检验》", 31 August 2015, 中国医药科技出版社 *

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Application publication date: 20171020