CN111318046A - Integrated dioxin distillation extraction instrument and use method thereof - Google Patents
Integrated dioxin distillation extraction instrument and use method thereof Download PDFInfo
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- CN111318046A CN111318046A CN202010351723.1A CN202010351723A CN111318046A CN 111318046 A CN111318046 A CN 111318046A CN 202010351723 A CN202010351723 A CN 202010351723A CN 111318046 A CN111318046 A CN 111318046A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/16—Retorts
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention belongs to the technical field of toxic gas detection devices, and particularly relates to an integrated dioxin distillation and extraction instrument and a using method thereof. The invention provides an integrated dioxin distillation extraction apparatus, which comprises a shell and a plurality of extraction units positioned in the shell, wherein each extraction unit comprises the following components in sequence from bottom to top: the solvent bottle, the cable lifting device and the condensing device are connected with the upper part of the cable lifting device; a cooling water pipeline of the condensing device is respectively connected with a cooling water circulating water pump and a cooling water tank; the lower part of the solvent bottle is provided with a heating device. For the sampling device of the ambient air and industrial waste gas sampling instrument, the sampling device can be directly placed in the cable lifting device for experiment without sample transfer, and the accuracy of the experiment is improved. In addition, the invention integrates heating, distillation, extraction and cooling water circulation, can be widely applied to sample analysis and experiments of food, medicines, environmental samples and the like, and is particularly suitable for the pretreatment process of sample detection of dioxin and the like.
Description
Technical Field
The invention belongs to the technical field of toxic gas detection devices, and particularly relates to an integrated dioxin distillation extraction apparatus and a using method of the extraction apparatus.
Background
At present, the environmental protection trade does not have the pretreatment experimental apparatus who is applicable to dioxin in detection ring border atmosphere and industrial waste gas, and many analysis laboratories are the simple and easy experimental apparatus who builds temporarily, and occupation space is big, and degree of automation is low, operates inconveniently, from causing experimental work efficiency to hang down.
For example, the utility model patent document discloses a fat measuring instrument, which has no built-in cooling water circulation system, needs external cooling water circulation, and causes large occupied volume of the instrument and equipment and troublesome operation; the volume of the solvent cup is less than 100 ml, and 300 ml of organic solvent is often needed for extracting dioxin in the environmental atmosphere and industrial waste gas; the fat determinator is plane heating, the solvent cup is cylindrical and is in a water cup shape, the heating efficiency is low, and the solvent is heated unevenly; the fat determinator is a two-layer structure, namely a solvent cup and a condensation component, and an extraction part is embedded between the solvent cup and the condensation component, so that the experiment of a large-volume sample cannot be carried out. Therefore, it is necessary to improve the above structure, and to invent an integrated dioxin distillation and extraction apparatus which integrates distillation and extraction, and has a small volume and a high degree of automation.
Disclosure of Invention
In order to solve the technical problems, the invention provides an integrated dioxin distillation and extraction instrument which integrates distillation and extraction, has small volume, high automation degree and convenient operation, and does not need special persons to watch during operation.
Integration dioxin distillation extraction appearance includes the casing to and be located the inside a plurality of extraction units of casing, the structure of every extraction unit is the same, every extraction unit is from bottom to top in proper order: the device comprises a solvent bottle, a cable lifting device connected with the upper part of the solvent bottle, and a condensing device connected with the upper part of the cable lifting device; the condensing device comprises condensing bottles, adjacent condensing bottles are connected in series through a pipeline, a cooling circulating water outlet of the last condensing bottle is connected with a cooling water tank, a cooling circulating water inlet of the first condensing bottle is connected with a cooling water circulating water pump, and the compression refrigerating device is also connected with the cooling water tank; the lower part of the solvent bottle is provided with a heating device.
The heating device is preferably a ceramic heating device, the ceramic heating device comprises a ceramic heater shell and a plurality of ceramic heaters positioned in the ceramic heater shell, and each ceramic heater is positioned below each corresponding solvent bottle and matched with the solvent bottle;
preferably, the ceramic heater is externally provided with a heat insulation material layer.
And a display control device is arranged on one side of the outer surface of the shell and is electrically connected with the ceramic heating device and the compression refrigerating device.
The solvent bottle and the cable lifting device are connected through a spherical grinding port which is positioned above the solvent bottle and matched with the solvent bottle and are fixed by a spherical grinding port clamp;
preferably, the cable lifting device comprises a cable lifting pipe and a cable lifting dropping liquid pipe, and the cable lifting pipe and the cable lifting dropping liquid pipe are connected through a cable lifting pipe air inlet pipeline; the lower end of the rope lifting pipe air inlet pipeline is communicated with the lower part of the rope lifting pipe, and the lower end of the rope lifting pipe air inlet pipeline is communicated with the solvent bottle;
preferably, the lower part of the cable lifting pipe is communicated with a cable lifting pipe liquid discharge pipeline, and the lower part of the cable lifting pipe liquid discharge pipeline is communicated with the solvent bottle;
the cable lifting device is connected with the condensing device through a plane flange grinding port and is fixed by a plane flange grinding port clamp;
preferably, the cable body device is fixed on the shell through a cable lifting pipe fixing clip.
A cooling water cavity, a condensation tube cavity and a condensation bottle vacuum cavity are arranged in the condensation bottle; a cooling circulating water outlet is arranged above the condensation bottle, and a condensation bottle exhaust port is arranged at the upper part of the condensation tube cavity; the cooling water cavity is connected with a cooling water circulating water pump through a cooling circulating water inlet;
the compression refrigeration device comprises a refrigeration compressor, an evaporator and a condenser; wherein the refrigeration compressor, the evaporator and the condenser are connected through pipelines to form a closed loop;
the compression refrigerating device is connected with the cooling water tank and carries out cooling treatment on the cooling water tank.
A guide device is arranged outside the condensing device, the guide device is cylindrical, the outer wall of the guide device is connected with the shell, and a buffer layer is arranged between the inner wall of the guide device and the condensing bottle;
preferably, the buffer layer is a rubber pad;
preferably, the condensation bottle is positioned in the guide device and can move up and down along the axial direction of the guide device;
the solvent bottle is provided with a solvent bottle spherical ground mouth;
preferably, the upper part of the air inlet pipeline of the rope lifting pipe is provided with a small conical grinding opening;
preferably, the lower part of the rope lifting pipe is provided with a rope lifting pipe air inlet spherical grinding opening;
the left end of the rope-lifting dropping liquid pipe is matched and connected with the small conical grinding opening, and the rope-lifting dropping liquid pipe is in a 7 shape.
The use method of the integrated dioxin distillation and extraction instrument comprises the following steps:
the solvent in the solvent bottle is heated by a ceramic heating device in the solvent bottle, and enters the rope lifting pipe along a rope lifting pipe air inlet pipeline and a rope lifting dropping liquid pipe on the rope lifting pipe, at the moment, the condensing device provides circulating cooling water for the extraction process, the condensed solvent flows into the rope lifting pipe and soaks the sample in the sample container and reacts with the sample, and the solvent containing the sample to be detected generates siphonage after accumulating in the rope lifting pipe, so that the solvent is discharged into the solvent bottle through a liquid discharge pipeline of the rope lifting pipe; the gaseous solvent enters the condensing device, flows into the lifting rope pipe after being condensed, soaks the sample in the sample container and reacts with the sample, and the solvent containing the sample to be detected generates siphonage after accumulating in the lifting rope pipe so as to be discharged into the solvent bottle through a liquid discharge pipeline of the lifting rope pipe; the above steps are repeated until the sample to be tested is completely extracted into the solvent bottle. The extraction instrument provided by the invention has the following remarkable advantages:
(1) the device integrates heating, distillation, extraction and cooling water circulation, and has high automation degree and convenient operation;
(2) for the sampling devices of the ambient air and industrial waste gas sampling instrument, the sampling devices can be directly placed in the cable lifting device for experiment without sample transfer, so that the accuracy of the experiment is improved;
(3) the heating device adopts a ceramic heating device consisting of a plurality of ceramic heaters, the power and the working time of the heating device can be controlled independently, the control precision is high, and the experimental operation is convenient;
(4) the compression refrigerating device is provided with a cooling circulating water system, so that water resources are saved.
Drawings
Fig. 1 is a schematic front structural view of fig. 1 according to embodiment 1 of the present invention;
FIG. 2 is a schematic diagram of embodiment 1 of the present invention;
FIG. 3 is a schematic view of the structure of the solvent bottle of example 1;
FIG. 4 is a schematic view of a ceramic heating apparatus according to example 1 of the present invention;
FIG. 5 is a schematic view of a lift device according to embodiment 1 of the present invention;
FIG. 6 is a schematic view of a condensing apparatus according to embodiment 1 of the present invention;
FIG. 7 is a schematic structural view of example 2 of the present invention;
in the figure: 1-shell, 2-solvent bottle, 3-cooling water tank, 4-spherical ground clamp, 5-lifting pipe, 6-sample container, 7-lifting pipe fixing clamp, 8-lifting dropping liquid pipe, 9-plane flange ground clamp, 10-condensation bottle, 11-guiding device, 13-cooling water circulating water pump, 14-display control device, 15-ceramic heater, 16-solvent, 17-lifting pipe drainage pipeline, 18-lifting pipe air inlet pipeline, 19-condensation bottle cooling circulating water inlet, 20-condensation bottle cooling circulating water drainage port, 21-condensation bottle exhaust port, 22-condensation bottle vacuum cavity, 23-condensation bottle cooling water cavity, 24-condensation bottle condensation cavity, 25-refrigeration compressor, 26-evaporator, 27-condenser, 28-ceramic heater shell, 29-thermal insulation material, 30-rope lifting pipe air inlet spherical ground port, 31-rope lifting pipe air outlet plane flange ground port, 32-small conical ground port, 33-condensation bottle air inlet plane flange ground port, 35-rubber pad, 42-solvent bottle spherical ground port, 43-ceramic heating device, 44-condensation device, 45-rope lifting device and 46-compression refrigeration device.
Detailed Description
The present invention will now be further described with reference to specific embodiments in order to enable those skilled in the art to better understand the present invention.
Example 1
The invention provides an integrated dioxin distillation extraction apparatus, which comprises a shell 1 and a plurality of extraction units positioned in the shell 1, wherein the structure of each extraction unit is the same, and each extraction unit is sequentially from bottom to top: the solvent bottle 2, a rope lifting device 45 connected with the upper part of the solvent bottle 2, and a condensing device 44 connected with the upper part of the rope lifting device 45; the condensing device 44 comprises condensing bottles 10, adjacent condensing bottles 10 are connected in series through a pipeline, a cooling circulating water outlet of the last condensing bottle 10 is connected with the cooling water tank 3, a cooling circulating water inlet of the first condensing bottle 10 is connected with the cooling water circulating water pump 13, and the compression refrigerating device 46 is connected with the cooling water tank 3; the lower part of the solvent bottle 2 is provided with a heating device.
The heating device is a ceramic heating device 43, the ceramic heating device 43 comprises a ceramic heater shell 28 and a plurality of ceramic heaters 15 positioned in the ceramic heater shell 28, and each ceramic heater 15 is positioned below each corresponding solvent bottle 2 and matched with the solvent bottle 2;
the ceramic heater 15 has a layer of insulating material 29 on the outside for insulation.
The display control device 14 is arranged on one side of the outer surface of the shell 1, and the display control device 14 is electrically connected with the ceramic heating device 43 and the compression refrigerating device 46.
The solvent bottle 2 and the rope lifting device 45 are connected through a matched spherical ground opening positioned above the solvent bottle 2 and are fixed by a spherical ground opening clamp 4;
the cable lifting device 45 comprises a cable lifting pipe 5 and a cable lifting dropping liquid pipe 8, and the cable lifting pipe 5 and the cable lifting dropping liquid pipe 8 are connected through a cable lifting pipe air inlet pipeline 18; the lower end of the rope lifting pipe air inlet pipeline 18 is communicated with the lower part of the rope lifting pipe 5, and the lower end of the rope lifting pipe air inlet pipeline 18 is communicated with the solvent bottle 2;
the lower part of the rope lifting pipe 5 is communicated with a rope lifting pipe liquid discharge pipeline 17, and the lower part of the rope lifting pipe liquid discharge pipeline 17 is communicated with the solvent bottle 2;
the cable lifting device 45 is fixed to the housing 1 by means of a cable lifting tube fixing clip 7.
A condensation bottle cooling water cavity 23, a condensation bottle condensation tube cavity 24 and a condensation bottle vacuum cavity 22 are arranged in the condensation bottle 10; a condensation bottle cooling circulating water outlet 20 is arranged above the condensation bottle 10, and a condensation bottle exhaust port 21 is arranged at the upper part of a condensation bottle condensation tube cavity 24; the cooling water cavity 23 of the condensation bottle is connected with a cooling water circulating water pump 13 through a cooling circulating water inlet 19;
the compression refrigeration device 46 comprises a refrigeration compressor 25, an evaporator 26 and a condenser 27; wherein, the refrigeration compressor 25, the evaporator 26 and the condenser 27 are connected by pipelines to form a closed loop;
the compression refrigeration device 46 is connected to the cooling water tank 3 and cools the cooling water in the cooling water tank 3.
A guide device 11 is arranged outside the condensing device 44, the guide device 11 is cylindrical, the outer wall of the guide device 11 is connected with the shell 1, and a buffer layer is arranged between the inner wall and the condensing bottle 10; the buffer layer is a rubber pad 35 and is used for preventing the condensation bottle 10 from colliding with the guide device 11 so as to break the condensation bottle 10;
the condensation bottle 10 is positioned in the guide device 11 and can move up and down along the axial direction of the guide device 11;
the lower part of the condensation bottle 10 is provided with a gas inlet plane flange ground port 33, and the upper top of the rope lifting pipe 5 is provided with a rope lifting pipe gas outlet plane flange ground port 31; so that the cable lifting device 45 and the condensing device 44 are relatively fixed through the planar flange grinding clamp 9;
the solvent bottle 2 is provided with a solvent bottle spherical ground 42;
the upper part of the rope lifting pipe air inlet pipeline 18 is provided with a small conical grinding opening 32;
the lower part of the rope lifting pipe 5 is provided with a rope lifting pipe air inlet spherical grinding opening 30;
the left end of the rope lifting dropping liquid pipe 8 is connected with a small conical grinding opening 32 in a matching way, and the rope lifting dropping liquid pipe 8 is in a 7 shape. The grinding opening structures have the effect of enabling the air tightness between two connected parts to be better, thereby being beneficial to extraction and further improving the accuracy of detection results.
The integrated dioxin distillation and extraction apparatus provided by the embodiment 1 and the using method thereof comprise the following steps:
the solvent 16 in the solvent bottle 2 is heated by a ceramic heating device 43 in the solvent bottle 2, enters the rope lifting pipe 5 along the rope lifting pipe air inlet pipeline 18 and the rope lifting dropping liquid pipe 8 on the rope lifting pipe 5, at the moment, a condensing device 44 provides circulating cooling water for the extraction process, the condensed solvent flows into the rope lifting pipe 5 and soaks and reacts with the sample in the sample container 6, and the solvent containing the sample to be detected generates a siphon phenomenon after accumulating in the rope lifting pipe so as to be discharged into the solvent bottle 2 through a liquid discharge pipeline 17 of the rope lifting pipe; the gaseous solvent enters the condensing device 44, flows into the lifting pipe 5 after being condensed, soaks and reacts with the sample in the sample container 6, and the solvent containing the sample to be detected generates siphonage after accumulating in the lifting pipe 5 so as to be discharged into the solvent bottle 2 through the liquid discharge pipeline 17 of the lifting pipe 5; the above-described steps are repeated until the sample to be tested is completely extracted into the solvent bottle 2.
Example 2
The difference from the embodiment 1 is that the cooling water circulation system without compressor refrigeration is externally connected with cooling water. The cooling water enters the condensation component 44 through the instrument water inlet 47 and is discharged through the instrument water outlet 48, and the rest of the technical structure is the same as that of the embodiment 1, and the partial structure of the embodiment 2 is shown in fig. 7.
Claims (8)
1. Integration dioxin distillation extraction appearance, its characterized in that, the extraction appearance include casing (1) to and be located the inside a plurality of extraction units of casing (1), every extraction unit's structure is the same, every extraction unit is from bottom to top in proper order: the device comprises a solvent bottle (2), a rope lifting device (45) connected with the upper part of the solvent bottle (2), and a condensing device (44) connected with the upper part of the rope lifting device (45); the condensing device (44) comprises condensing bottles (10), adjacent condensing bottles (10) are connected in series through a pipeline, a cooling circulating water outlet of the last condensing bottle (10) is connected with the cooling water tank (3), and a cooling circulating water inlet of the first condensing bottle (10) is connected with the cooling water circulating water pump (13); the cooling water circulating water pump (13) is also connected with a compression refrigerating device (46), and the lower part of the solvent bottle (2) is provided with a heating device.
2. The integrated dioxin distillation and extraction apparatus of claim 1, wherein the heating device is a ceramic heating device (43), the ceramic heating device (43) comprises a ceramic heater housing (28) and a plurality of ceramic heaters (15) positioned in the ceramic heater housing (28), and each ceramic heater (15) is positioned below each corresponding solvent bottle (2) and matched with the solvent bottle (2);
preferably, the ceramic heater (15) is externally provided with a heat insulating material layer (29).
3. The integrated dioxin distillation and extraction apparatus as claimed in claim 1, wherein the display control device (14) is provided on one side of the outer surface of the casing (1), and the display control device (14) is electrically connected with the ceramic heating device (43) and the compression refrigeration device (46).
4. The integrated dioxin distillation and extraction apparatus as claimed in claim 1, wherein the solvent bottle (2) and the rope-lifting device (45) are connected through a matched spherical ground which is positioned above the solvent bottle (2) and fixed by a spherical ground clamp (4);
preferably, the cable lifting device (45) comprises a cable lifting pipe (5) and a cable lifting dropping liquid pipe (8), and the cable lifting pipe (5) and the cable lifting dropping liquid pipe (8) are connected through a cable lifting pipe air inlet pipeline (18); the lower end of the rope lifting pipe air inlet pipeline (18) is communicated with the lower part of the rope lifting pipe (5), and the lower end of the rope lifting pipe air inlet pipeline (18) is communicated with the solvent bottle (2);
preferably, the lower part of the cable lifting pipe (5) is communicated with a cable lifting pipe drainage pipeline (17), and the lower part of the cable lifting pipe drainage pipeline (17) is communicated with the solvent bottle (2);
the cable lifting device (45) and the condensing device (44) are relatively fixed through a plane flange ground clamp (9);
preferably, the cable lifting device (45) is fixed on the shell (1) through a cable lifting pipe fixing clip (7).
5. The integrated dioxin distillation and extraction instrument according to claim 1, wherein the condensing flask (10) is internally provided with a condensing flask cooling water cavity (23), a condensing flask condensing tube cavity (24) and a condensing flask vacuum cavity (22); a condensation bottle cooling circulating water outlet (20) is arranged above the condensation bottle (10), and a condensation bottle exhaust port (21) is arranged at the upper part of a condensation bottle condensation tube cavity (24); the cooling water cavity (23) of the condensation bottle is connected with a cooling water circulating water pump (13) through a cooling circulating water inlet (19);
the compression refrigeration device (46) comprises a refrigeration compressor (25), an evaporator (26) and a condenser (27); wherein the cold compressor (25), the evaporator (26) and the condenser (27) are connected through pipelines to form a closed loop;
the compression refrigeration device (46) is connected with the cooling water tank (3) and cools the cooling water tank (3).
6. The integrated dioxin distillation and extraction apparatus as claimed in claim 1, wherein the condensing unit (44) is externally provided with a guide unit (11), the guide unit (11) has a cylindrical shape, the outer wall thereof is connected to the casing (1), and a buffer layer is provided between the inner wall thereof and the condensing flask (10);
preferably, the buffer layer is a rubber pad (35);
preferably, the condensation bottle (10) is positioned in the guide device (11) and can move up and down along the axial direction of the guide device (11);
preferably, the lower part of the condensation bottle (10) is provided with an air inlet plane flange ground port (33).
7. The integrated dioxin distillation and extraction apparatus of claim 1, wherein the solvent bottle (2) has a solvent bottle ball mill mouth (42);
preferably, the upper part of the rope lifting pipe air inlet pipeline (18) is provided with a small conical grinding opening (32);
preferably, the lower part of the rope lifting pipe (5) is provided with a rope lifting pipe air inlet spherical grinding opening (30);
the upper top of the rope lifting pipe (5) is provided with a rope lifting pipe air outlet plane flange ground mouth (31);
the left end of the rope lifting dropping liquid pipe (8) is connected with the small conical grinding opening (32) in a matching way, and the rope lifting dropping liquid pipe (8) is in a 7 shape.
8. The method for using the integrated dioxin distillation and extraction apparatus in claim 1 comprises the following steps:
the solvent (16) in the solvent bottle (2) is heated by a ceramic heating device (43) in the solvent bottle (2), enters the lifting pipe (5) along a lifting pipe air inlet pipeline (18) and a lifting dropping liquid pipe (8) on the lifting pipe (5), at the moment, a condensing device (44) provides circulating cooling water for the extraction process, the condensed solvent flows into the lifting pipe (5) and soaks and reacts with the sample in the sample container (6), and the solvent containing the sample to be detected generates a siphon phenomenon after accumulating in the lifting pipe so as to be discharged into the solvent bottle (2) through a liquid discharge pipeline (17) of the lifting pipe; the gaseous solvent enters a condensing device (44), flows into the lifting pipe (5) after being condensed, soaks the sample in the sample container (6) and reacts with the sample, and the solvent containing the sample to be detected generates a siphonage phenomenon after accumulating in the lifting pipe (5) so as to be discharged into the solvent bottle (2) through a liquid discharge pipeline (17) of the lifting pipe (5); the above steps are repeated until the sample to be detected is completely extracted into the solvent bottle (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010351723.1A CN111318046A (en) | 2020-04-28 | 2020-04-28 | Integrated dioxin distillation extraction instrument and use method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010351723.1A CN111318046A (en) | 2020-04-28 | 2020-04-28 | Integrated dioxin distillation extraction instrument and use method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112121460A (en) * | 2020-10-01 | 2020-12-25 | 高建新 | A extraction subassembly for tea-oil camellia seed cleaning powder |
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2020
- 2020-04-28 CN CN202010351723.1A patent/CN111318046A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112121460A (en) * | 2020-10-01 | 2020-12-25 | 高建新 | A extraction subassembly for tea-oil camellia seed cleaning powder |
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