CN204034306U - A kind of modified SDE method increasing Liquid-liquid Extraction Processes - Google Patents
A kind of modified SDE method increasing Liquid-liquid Extraction Processes Download PDFInfo
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- CN204034306U CN204034306U CN201420424320.5U CN201420424320U CN204034306U CN 204034306 U CN204034306 U CN 204034306U CN 201420424320 U CN201420424320 U CN 201420424320U CN 204034306 U CN204034306 U CN 204034306U
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Abstract
The utility model is specifically related to a kind of Simultaneous distillation-extraction instrument.This device principal character is to be provided with a liquid-liquid extraction bottle in the middle part of U-shaped layering return duct, and liquid-liquid extraction bottle bottle wall top is provided with upper shed, and bottom is provided with under shed; Extraction condensation chamber closed downwards, and below side, be provided with condensation opening, condensation opening is connected by entering pipeline with the under shed of liquid-liquid extraction bottle; The top of U-shaped layering return duct is provided with reflux opening, reflux opening is connected by the pipeline that sets out with the upper shed of liquid-liquid extraction bottle, the upper shed of condensation opening and liquid-liquid extraction bottle is in the same plane, and the under shed of reflux opening and liquid-liquid extraction bottle is in the same plane.The utility model is the improvement done on existing SDE method basis, by improving, increasing Liquid-liquid Extraction Processes, can improve effect of extracting and the extraction efficiency of organic extraction solvent preferably, thus have good applicability and generalization.
Description
Technical field
The utility model is specifically related to a kind of Simultaneous distillation-extraction instrument, and this instrument, carrying out, in the Simultaneous distillation-extraction course of work, adding Liquid-liquid Extraction Processes, can effectively improve organic extraction effect and extraction efficiency.
Background technology
To the analysis of volatilization, half volatile flavor matter in tobacco, a kind of Simultaneous distillation-extraction instrument of normal employing equipment, the composition of rising with water azeotropic in tobacco can extract and be transferred in organic phase by this instrument, and then utilizes other equipment to be further analyzed the volatile substance in these tobaccos.
The Simultaneous distillation-extraction instrument used in prior art, the extraction that extract treated by extractant depends on the extraction under gaseous state, and extraction component is limited, is thus necessary to improve its effect of extracting further.
Summary of the invention
The utility model object is to provide a kind of modified SDE method, and this device adds the Liquid-liquid Extraction Processes that organic solvent treats extract, can effectively improve organic extraction effect and extraction efficiency.
Technical solution adopted in the utility model is as follows.
Increase a modified SDE method for Liquid-liquid Extraction Processes, comprise two distil containers, 1, two distillation cascades 2, hybrid extraction condensation chamber 3, U-shaped layering return duct 4, tap hole 5, two backflow arm 6, two siphon graded tubes 7, two inverted U-shaped siphon arms 8;
Two distillation cascade 2 one end are respectively inserted on a distil container 1, and the other end is connected to hybrid extraction condensation chamber 3 upper end;
Hybrid extraction condensation chamber 3 lower end is connected with U-shaped layering return duct 4; U-shaped layering return duct 4 is communicated with distillation cascade 2 respectively by backflow arm 6; The backflow arm 6 be connected with distillation cascade 2 is provided with siphon graded tube 7;
Siphon graded tube 7 is connected with distillation cascade 2 by inverted U-shaped siphon arm 8, and inverted U-shaped siphon arm 8 tip position is lower than the siphon graded tube 7 graded tube graduation mark upper limit;
The tap hole 5 of a band piston is provided with bottom U-shaped layering return duct 4;
Be provided with a liquid-liquid extraction bottle 9 in the middle part of U-shaped layering return duct 4, liquid-liquid extraction bottle 9 bottles of wall tops are provided with upper shed 12, and bottom is provided with under shed 13;
Below extraction condensation chamber 3,14 places close, and below side, be provided with condensation opening 10, and condensation opening 10 is connected by entering pipeline with the under shed 13 of liquid-liquid extraction bottle 9;
The top of U-shaped layering return duct 4 is provided with reflux opening 11, and reflux opening 11 is connected by the pipeline that sets out with the upper shed 12 of liquid-liquid extraction bottle 9;
The upper shed 12 of condensation opening 10 and liquid-liquid extraction bottle 9 is in the same plane, and reflux opening 11 is in the same plane with the under shed 13 of liquid-liquid extraction bottle 9.
The modified SDE method of described increase Liquid-liquid Extraction Processes, distillation cascade 2 adopts vacuum double structure.
The modified SDE method of described increase Liquid-liquid Extraction Processes, liquid-liquid extraction bottle 9 is round-bottomed flask; Be added with magnetic stir bar in liquid-liquid extraction bottle 9, liquid-liquid extraction bottle 9 is placed on magnetic stirring apparatus.
When the utility model uses, organic extraction solvent is filled in a distil container 1, the organic extraction solvent held volatilizees and enters in extraction condensation chamber 3 under suitable temperature condition, another volatile ingredient filled in the distil container 1 of thing to be extracted also evaporates in extraction condensation chamber 3 under suitable temperature condition, in extraction condensation chamber 3, the easily soluble component that organic extraction solvent is treated in extract realizes extraction.In prior art, organic extraction solvent is treated the extraction of related substances in extract and is depended on and carry out under gaseous state in extraction condensation chamber 3, this extraction mode, and the efficiency of extraction, effect of extracting are by restriction to a certain extent.The utility model is by setting up liquid liquid extraction plant 9, and in extraction condensation chamber 3, condensed gas is not directly be separated, but enters in liquid liquid extraction plant 9, by setting up magnetic stir bar in liquid liquid extraction plant 9, improves liquid-liquid extraction efficiency.Along with condensate liquid constantly enters in liquid liquid extraction plant 9, the solution after liquid-liquid extraction refluxes again to enter in SDE method and carries out later separation.
The utility model is the improvement done on existing SDE method basis, by improving, increasing Liquid-liquid Extraction Processes, can improve effect of extracting and the extraction efficiency of organic extraction solvent preferably, thus have good applicability and generalization.
Accompanying drawing explanation
Fig. 1 is the structural representation of modified SDE method provided by the utility model.
Detailed description of the invention
Below in conjunction with embodiment, explanation is further explained to the utility model.
Embodiment
As shown in Figure 1, the modified SDE method of increase Liquid-liquid Extraction Processes provided by the utility model, comprises two distil containers, 1, two distillation cascades 2, hybrid extraction condensation chamber 3, U-shaped layering return duct 4, tap hole 5, two backflow arm 6, two siphon graded tubes 7, two inverted U-shaped siphon arms 8;
Two distillation cascade 2 one end are respectively inserted on a distil container 1, and the other end is connected to hybrid extraction condensation chamber 3 upper end;
Hybrid extraction condensation chamber 3 lower end is connected with U-shaped layering return duct 4; U-shaped layering return duct 4 is communicated with distillation cascade 2 respectively by backflow arm 6; The backflow arm 6 be connected with distillation cascade 2 is provided with siphon graded tube 7;
Siphon graded tube 7 is connected with distillation cascade 2 by inverted U-shaped siphon arm 8, and inverted U-shaped siphon arm 8 tip position is lower than the siphon graded tube 7 graded tube graduation mark upper limit;
The tap hole 5 of a band piston is provided with bottom U-shaped layering return duct 4;
Be provided with a liquid-liquid extraction bottle 9 in the middle part of U-shaped layering return duct 4, liquid-liquid extraction bottle 9 bottles of wall tops are provided with upper shed 12, and bottom is provided with under shed 13;
Below extraction condensation chamber 3,14 places close, and below side, be provided with condensation opening 10, and condensation opening 10 is connected by entering pipeline with the under shed 13 of liquid-liquid extraction bottle 9;
The top of U-shaped layering return duct 4 is provided with reflux opening 11, and reflux opening 11 is connected by the pipeline that sets out with the upper shed 12 of liquid-liquid extraction bottle 9;
The upper shed 12 of condensation opening 10 and liquid-liquid extraction bottle 9 is in the same plane, and reflux opening 11 is in the same plane with the under shed 13 of liquid-liquid extraction bottle 9.
Distillation cascade 2 adopts vacuum double structure.
Liquid-liquid extraction bottle 9 is round-bottomed flask; Be added with magnetic stir bar in liquid-liquid extraction bottle 9, liquid-liquid extraction bottle 9 is placed on magnetic stirring apparatus.
For the Simultaneous distillation-extraction process that certain is concrete, illustrate the workflow of SDE method provided by the utility model.
(1) raw material preparation, gets after a certain single grade pipe tobacco dries 1.0h in 45 DEG C of baking ovens and pulverizes, and crosses 80 mesh sieve, mixes, seal for subsequent use.
(2) accurately take 20.0000g offal in step (1) and in the round-bottomed flask of 1000mL, add 500mL distilled water, this i.e. one of them distil container, accurately takes 80mL carrene and adds in 100mL round-bottomed flask, and this i.e. another distil container.
(3) under 10 DEG C of condensation temperatures, Simultaneous distillation-extraction 2 h is carried out; During Simultaneous distillation-extraction, fill carry out of distil container along with heating process of pipe tobacco, in pipe tobacco, volatile substances extracts in condensation chamber 3 along with steam enters; Fill carry out of distil container along with heating process of organic extraction solvent, organic extraction solvent chloroform also volatilizees and enters in extraction condensation chamber 3; In extraction condensation chamber 3, organic extraction solvent chloroform extracts volatile substances mixing in pipe tobacco, along with the cooling effect of condensation chamber 3, gas cool gradually concurrent raw food coagulate, condensed liquid to enter in liquid liquid extraction plant 9 and carries out further liquid-liquid extraction, be provided with magnetic stir bar in liquid liquid extraction plant 9 and be placed on magnetic stirring apparatus, this setting can improve the mixing degree of extractant and thing to be extracted and accelerate extraction progress.Along with entering increasing of liquid in liquid liquid extraction plant 9, the liquid after extraction enters SDE method again and is further separated.
(4) after organic extraction, add 4.0g anhydrous sodium sulfate drying and spend the night, be concentrated into 1mL after filtration in organic phase, this is sample to be analyzed.
Under the same terms, for the SDE method do not improved, carry out the distillation extraction under the same terms, prepare sample to be analyzed.
GC-MS analysis is carried out to sample to be analyzed:
(1) GC condition: carrier gas, helium; Flow velocity, 1mL/min; Sample size, 1 μ L; Split ratio, 10:1; Chromatographic column, DB-5MS capillary column (μm i.d. × 0.25,30.0m × 250 μm d.f.); Temperature programming, 40 DEG C keep 3.0min, then rise to 280 DEG C with 4 DEG C/min speed, keep 20.0min;
(2) MS condition: transmission line temperature, 230 DEG C; Ionization electric energy, 70eV; Quadrupole rod temperature, 150 DEG C; EI ion source temperature, 230 DEG C; Scanning of the mass spectrum scope, 20 ~ 400amu.
The qualitative analysis of Nist08 picture library MS manual search is adopted according to molecular weight and mass spectral fragments collection of illustrative plates.
Carry out integration to sample chromatogram peak respectively, the peak area ratio according to tie substance judges extraction efficiency, the results are shown in following table.
Note: A is the modified SDE method of increase Liquid-liquid Extraction Processes provided by the utility model and the peak area ratio of the SDE method tie substance do not improved, and namely A=improves rear peak area ÷ and do not improve peak area.
Detect data as can be seen from table, after adopting the utility model, the extraction efficiency for main matter has lifting in various degree, shows good effect of extracting, achieves goal of the invention of the present utility model preferably.
Claims (3)
1. one kind increases the modified SDE method of Liquid-liquid Extraction Processes, it is characterized in that, this device comprises two distil containers (1), two distillation cascades (2), hybrid extraction condensation chamber (3), U-shaped layering return duct (4), tap hole (5), two backflows arm (6), two siphon graded tubes (7), two inverted U-shaped siphon arms (8);
Two distillation cascade (2) one end are respectively inserted on a distil container (1), and the other end is connected to hybrid extraction condensation chamber (3) upper end;
Hybrid extraction condensation chamber (3) lower end is connected with U-shaped layering return duct (4); U-shaped layering return duct (4) is communicated with distillation cascade (2) respectively by backflow arm (6); The backflow arm (6) be connected with distillation cascade (2) is provided with siphon graded tube (7);
Siphon graded tube (7) is connected with distillation cascade (2) by inverted U-shaped siphon arm (8), and inverted U-shaped siphon arm (8) tip position is lower than siphon graded tube (7) the graded tube graduation mark upper limit;
U-shaped layering return duct (4) bottom is provided with the tap hole (5) of a band piston;
U-shaped layering return duct (4) middle part is provided with a liquid-liquid extraction bottle (9), and liquid-liquid extraction bottle (9) bottle wall top is provided with upper shed (12), and bottom is provided with under shed (13);
(14) place, extraction condensation chamber (3) below closes, and below side, be provided with condensation opening (10), and condensation opening (10) is connected by entering pipeline with the under shed (13) of liquid-liquid extraction bottle (9);
The top of U-shaped layering return duct (4) is provided with reflux opening (11), and reflux opening (11) is connected by the pipeline that sets out with the upper shed (12) of liquid-liquid extraction bottle (9);
The upper shed (12) of condensation opening (10) and liquid-liquid extraction bottle (9) is in the same plane, and reflux opening (11) is in the same plane with the under shed (13) of liquid-liquid extraction bottle (9).
2. increase the modified SDE method of Liquid-liquid Extraction Processes as claimed in claim 1, it is characterized in that, distillation cascade (2) adopts vacuum double structure.
3. increase the modified SDE method of Liquid-liquid Extraction Processes as claimed in claim 1, it is characterized in that, liquid-liquid extraction bottle (9) is round-bottomed flask; Liquid-liquid extraction bottle is added with magnetic stir bar in (9), and liquid-liquid extraction bottle (9) is placed on magnetic stirring apparatus.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105344126A (en) * | 2015-10-10 | 2016-02-24 | 上海应用技术学院 | Simple low-consumption extraction apparatus for solvent in distillation product |
CN107201275A (en) * | 2017-06-22 | 2017-09-26 | 河北中烟工业有限责任公司 | A kind of continuous still extraction equipment |
CN109387590A (en) * | 2018-09-30 | 2019-02-26 | 江苏中烟工业有限责任公司 | The extraction element of chemical component and extraction, analysis method in cigarette core material |
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2014
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105344126A (en) * | 2015-10-10 | 2016-02-24 | 上海应用技术学院 | Simple low-consumption extraction apparatus for solvent in distillation product |
CN107201275A (en) * | 2017-06-22 | 2017-09-26 | 河北中烟工业有限责任公司 | A kind of continuous still extraction equipment |
CN107201275B (en) * | 2017-06-22 | 2023-04-28 | 河北中烟工业有限责任公司 | Continuous distillation extraction device |
CN109387590A (en) * | 2018-09-30 | 2019-02-26 | 江苏中烟工业有限责任公司 | The extraction element of chemical component and extraction, analysis method in cigarette core material |
CN109387590B (en) * | 2018-09-30 | 2021-12-24 | 江苏中烟工业有限责任公司 | Extraction device and extraction and analysis method for chemical components in cigarette core material |
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Address after: 450000 Yulin South Road, Henan, Zheng Dong, No. 16 South Road, Zhengzhou Patentee after: China Tobacco Henan Industrial Co., Ltd. Address before: 450000 Zhengzhou agricultural road, Henan, No. 29 Patentee before: China Tobacco Henan Industrial Co., Ltd. |