CN210269334U - High-flux high-temperature hydrolysis device - Google Patents
High-flux high-temperature hydrolysis device Download PDFInfo
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- CN210269334U CN210269334U CN201920757792.5U CN201920757792U CN210269334U CN 210269334 U CN210269334 U CN 210269334U CN 201920757792 U CN201920757792 U CN 201920757792U CN 210269334 U CN210269334 U CN 210269334U
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- pipe
- branch pipe
- combustion
- carrier gas
- temperature hydrolysis
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- 230000007062 hydrolysis Effects 0.000 title claims abstract description 29
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 29
- 238000002485 combustion reaction Methods 0.000 claims abstract description 45
- 239000012159 carrier gas Substances 0.000 claims abstract description 32
- 238000009833 condensation Methods 0.000 claims abstract description 18
- 230000005494 condensation Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 8
- 239000008236 heating water Substances 0.000 claims description 3
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 claims 1
- 230000004907 flux Effects 0.000 abstract description 10
- 238000005259 measurement Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000004255 ion exchange chromatography Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 229910001120 nichrome Inorganic materials 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model discloses a high flux high temperature hydrolysis unit relates to a pyrohydrolysis device, a plurality of combustion tubes pass multichannel heating furnace, the both ends of each combustion tube are entrance point and exit end respectively, the entrance point is equipped with the stopper, the injector is used for pushing into the combustion tube with the sample placer from the entrance point, all be provided with first branch pipe and second branch pipe on each combustion tube, each first branch pipe all is connected with vapor generation controlling means, each second branch pipe all is connected with carrier gas controlling means, condensation receiving arrangement includes the water-cooled generator, a plurality of condenser pipes and a plurality of receiving flask, the condenser pipe includes that inner tube and fixed cover locate the outer tube of inner tube outside, each exit end all with the access connection of an inner tube, the export of each inner tube lets in to a receiving flask in, the outer tube with the fraction in the water-cooled generator intercommunication is with the circulative cooling inner tube. The utility model provides a high flux high temperature hydrolysis unit can effectively improve sample pretreatment efficiency to improve sample measurement accuracy.
Description
Technical Field
The utility model relates to a high-temperature hydrolysis device, in particular to a high-flux high-temperature hydrolysis device.
Background
The existing methods for measuring fluorine and chlorine comprise X-ray fluorescence spectrometry, ion chromatography, ion selective electrode method and the like, and different methods have different requirements on the pretreatment of samples. At present, fluorine and chlorine of non-metal elements can be treated by a high-temperature hydrolysis method, and the fluorine and chlorine in the sample are extracted and absorbed by absorption liquid, and then measured by an instrument. At present, a conventional high-temperature hydrolysis device in a laboratory can only process one sample at a time, and the processing of one sample requires more than half an hour, so that the parallelism among the samples is poor, the sample processing speed is low, and the test precision is low.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a high flux high temperature hydrolysis unit to solve the problem that above-mentioned prior art exists, can effectively improve sample pretreatment efficiency, and improve sample test accuracy.
In order to achieve the above object, the utility model provides a following scheme:
the utility model provides a high-flux high-temperature hydrolysis device, which comprises a multi-channel heating furnace, a combustion pipe, a sample placer, a sample injector, a water vapor generation control device, a carrier gas control device and a condensation receiving device, wherein a plurality of combustion pipes pass through the multi-channel heating furnace, the two ends of each combustion pipe are respectively an inlet end and an outlet end, the inlet end is provided with a plug, the sample injector is used for pushing the sample placer into the combustion pipe from the inlet end, each combustion pipe is provided with a first branch pipe and a second branch pipe, the first branch pipe is arranged on the combustion pipe close to the inlet end, the second branch pipe is arranged on the combustion pipe between the first branch pipe and the inlet end, each first branch pipe is connected with the water vapor generation control device, the water vapor generation control device is used for producing fractions and controlling the fraction flow entering each first branch pipe, each second branch pipe is connected with the carrier gas control device, the carrier gas control device is used for controlling the flow of carrier gas entering each second branch pipe, the condensation receiving device comprises a water-cooling machine, a plurality of condensation pipes and a plurality of receiving bottles, each condensation pipe comprises an inner pipe and an outer pipe fixedly sleeved outside the inner pipe, each outlet end is connected with an inlet of one inner pipe, an outlet of each inner pipe is introduced into one receiving bottle, and the outer pipe is communicated with the water-cooling machine to circularly cool fractions in the inner pipes.
Preferably, the water vapor generation control device comprises a temperature control electric furnace, a water vapor generation bottle and a multi-way switch joint, the temperature control electric furnace is used for heating water in the water vapor generation bottle and controlling the temperature of the water in the water vapor generation bottle, an inlet pipe of the multi-way switch joint is connected with the water vapor generation bottle, an outlet pipe of the multi-way switch joint is connected with each first branch pipe, and a control switch is arranged on the outlet pipe of the multi-way switch joint.
Preferably, the carrier gas control device comprises a carrier gas bottle and a flow control valve, an inlet of the flow control valve is connected with an outlet of the carrier gas bottle, and an outlet of the flow control valve is connected with the second branch pipe.
Preferably, the combustion tube is a quartz combustion tube.
Preferably, the sample placer is a quartz boat.
Preferably, the sample injector is a nichrome sample injector.
Preferably, the outlet of the flow control valve is provided with a flow dividing device, and the flow dividing device uniformly divides the carrier gas to each second branch pipe.
Preferably, the condenser pipe is a spherical condenser pipe.
Preferably, a plurality of the outer pipes are connected in series and then communicated with the water cooler.
The utility model discloses for prior art gain following technological effect:
the utility model provides a high flux high temperature hydrolysis unit, through placing the test sample in the sample placer, and arrange the sample placer in the combustion tube, produce the fraction through vapor generation controlling means and let in the combustion tube with the fraction, carry out heat treatment to the sample in a plurality of combustion tubes in the multichannel heating furnace, the element pyrohydrolysis that awaits measuring in the sample, under the circulation effect of carrier gas, carry the fraction that contains the element that awaits measuring in the condenser tube among the condensation receiving arrangement, through the circulative cooling of water cooler to the fraction, collect the fraction after the condensation in the receiving flask, the absorption liquid in the receiving flask absorbs the element that awaits measuring, adopt selective electrode method or ion chromatography survey the content of the element that awaits measuring in the absorption liquid in the receiving flask, and calculate the content of the element that awaits measuring in obtaining every sample; adopt the utility model discloses a high flux high-temperature hydrolysis unit can once handle a plurality of samples, has reduced sample treatment time, improves sample pretreatment efficiency, handles a plurality of samples simultaneously, and the uniformity of each sample treatment condition can guarantee, can improve sample test accuracy.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural view of a medium-high flux high-temperature hydrolysis device according to the present invention;
FIG. 2 is a schematic structural view of a multi-channel heating furnace in the medium-high flux pyrohydrolysis device of the present invention;
in the figure: the device comprises a 1-multichannel heating furnace, a 2-combustion tube, a 3-sample placer, a 4-sample injector, a 5-steam generation control device, a 51-temperature control electric furnace, a 52-steam generation bottle, a 53-multi-way switch joint, a 6-carrier gas control device, a 61-carrier gas bottle, a 62-flow control valve, a 7-condensation receiving device, a 71-water cooler, a 72-condensation tube, a 721-inner tube, a 722-outer tube, a 73-receiving bottle, an 8-plug, a 9-first branch tube, a 10-second branch tube and an 11-shunt device.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
The utility model aims at providing a high flux high temperature hydrolysis unit to solve the problem that prior art exists, can effectively improve sample pretreatment efficiency, and improve sample test accuracy.
In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description.
As shown in fig. 1 to 2, the present embodiment provides a high-flux high-temperature hydrolysis apparatus, which includes a multi-channel heating furnace 1, combustion tubes 2, a sample holder 3, a sample injector 4, a water vapor generation control device 5, a carrier gas control device 6, and a condensation receiving device 7, wherein a plurality of combustion tubes 2 pass through the multi-channel heating furnace 1, two ends of each combustion tube 2 are respectively an inlet end and an outlet end, the inlet end is provided with a plug 8, the sample injector 4 is used for pushing the sample holder 3 into the combustion tube 2 from the inlet end, each combustion tube 2 is provided with a first branch tube 9 and a second branch tube 10, the first branch tube 9 is arranged on the combustion tube 2 near the inlet end, the second branch tube 10 is arranged on the combustion tube 2 between the first branch tube 9 and the inlet end, each first branch tube 9 is connected to the water vapor generation control device 5, the water vapor generation control device 5 is used for generating distillate and controlling the distillate flow entering each first branch tube 9, each second branch pipe 10 is connected with a carrier gas control device 6, the carrier gas control device 6 is used for controlling the flow of carrier gas entering each second branch pipe 10, the condensation receiving device 7 comprises a water-cooling machine 71, a plurality of condensation pipes 72 and a plurality of receiving bottles 73, each condensation pipe 72 comprises an inner pipe and an outer pipe fixedly sleeved outside the inner pipe, each outlet end is connected with an inlet of one inner pipe, an outlet of each inner pipe is introduced into one receiving bottle 73, and the outer pipe is communicated with the water-cooling machine 71 to circularly cool fractions in the inner pipe.
Placing a test sample in a sample placing device 3, pushing the sample placing device 3 into a combustion tube 2 by using a sample injector 4, generating fractions by using a water vapor generation control device 5, introducing the fractions into the combustion tube 2, heating the samples in the combustion tubes 2 in a multi-channel heating furnace 1, hydrolyzing elements to be detected in the samples at a high temperature, loading the fractions containing the elements to be detected into a condensation tube 72 under the circulation effect of carrier gas, circularly cooling the fractions by using a water cooler 71, collecting the condensed fractions into a receiving bottle 73, absorbing the elements to be detected by using absorption liquid in the receiving bottle 73, measuring the content of the elements to be detected in the absorption liquid in the receiving bottle 73 by using a selective electrode method or an ion chromatography, and calculating to obtain the content of the elements to be detected in each sample; adopt the utility model discloses a high flux high-temperature hydrolysis unit can once handle a plurality of samples, has reduced sample treatment time, improves sample pretreatment efficiency, handles a plurality of samples simultaneously, and the uniformity of each sample treatment condition can guarantee, can improve sample test accuracy.
The water vapor generation control device 5 comprises a temperature control electric furnace 51, a water vapor generation bottle 52 and a multi-way switch joint 53, the temperature control electric furnace 51 is used for heating water in the water vapor generation bottle 52 and controlling the water temperature in the water vapor generation bottle 52, an inlet pipe of the multi-way switch joint 53 is connected with the water vapor generation bottle 52, an outlet pipe of the multi-way switch joint 53 is connected with each first branch pipe 9, and a control switch is arranged on the outlet pipe of the multi-way switch joint 53. The water in the water vapor generation bottle 52 is heated by the temperature control electric furnace 51, the water temperature in the water vapor generation bottle 52 is controlled, the water vapor can uniformly enter each first branch pipe 9 through the outlet pipe of the multi-way switch joint 53, the water vapor flow in each first branch pipe 9 is ensured to be the same, and the consistent external treatment condition is ensured.
The carrier gas control means 6 includes a carrier gas cylinder 61 and a flow control valve 62, an inlet of the flow control valve 62 is connected to an outlet of the carrier gas cylinder 61, and an outlet of the flow control valve 62 is connected to the second branch pipe 10. The flow of carrier gas into the second manifold 10 can be controlled by the flow control valve 62 to meet the carrier gas flow requirements of the sample.
The combustion tube 2 is a quartz combustion tube, is high temperature resistant, and can ensure that a sample is heated to the high-temperature hydrolysis temperature.
The sample placer 3 is a quartz boat, is high temperature resistant, and can ensure that the sample is heated to the high-temperature hydrolysis temperature.
The sample injector 4 is a nichrome sample injector, and can push the sample placer 3 into the combustion tube 2 to heat when the combustion tube 2 is heated to the hydrolysis temperature.
The outlet of the flow control valve 62 is provided with a flow dividing device 11, and the flow dividing device 11 uniformly divides the carrier gas to each of the second branch pipes 10. Ensuring the same flow of carrier gas into each second branch pipe 10 and consistent external process conditions.
The condensing pipe 72 is a spherical condensing pipe, and the condensing effect on the distillate is better.
The outer pipes are connected in series and then communicated with the water cooler 71, and the outer pipes are connected in series and then communicated with the water cooler 71, so that fractions in the inner pipes can be circularly cooled.
In this embodiment, the combustion tube 2 is provided with two, all places a sample placer 3 in every combustion tube 2, and the exit end of every combustion tube 2 all with the access connection of the inner tube of a spherical condenser pipe, the export of the inner tube of each spherical condenser pipe all lets in to a receiving bottle 73 in, and two spherical condenser pipes's outer tube communicates with water-cooled machine 71 after establishing ties, can handle two samples that await measuring simultaneously.
Adopt the utility model provides a high flux high temperature hydrolysis unit to the fluorine content pretreatment process in the rock sample as follows:
(1) weighing 0.5g (accurate to 0.0002g) of rock powder sample and 0.5g of silicon dioxide powder, uniformly mixing, distributing in a quartz boat, covering with 0.5g of silicon dioxide powder, and simultaneously preparing five samples;
(2) taking 5mL of mixed absorption liquid of sodium bicarbonate and sodium carbonate into a receiving bottle 73, and preparing five absorption liquids at the same time;
(3) controlling the water temperature in the water vapor generation bottle 52 to be 90-96 ℃ by using a temperature control electric furnace 51, and controlling the flow rate of the distillate to be 1.0mL/min, so as to ensure that the flow rates entering the first branch pipes 9 are consistent;
(4) heating the multichannel heating furnace 1 to 1050 ℃, opening the flow control valve 62, and adjusting the flow entering each second branch pipe 10 to be 0.5-0.75 mL/min;
(5) opening a plug 8 at the inlet end of the combustion tube 2, pushing the quartz boat to the constant temperature position of the combustion tube 2, and plugging the plug 8;
(6) when the volume of the fraction received in the receiving bottle 73 is 25mL, the outlet end of the inner tube is flushed by a small amount of water, the fraction is combined in the fraction test solution, and the volume is increased to 30mL by water;
(7) the content of the fluorine element in the liquid contained in the receiving bottle 73 is measured by adopting a selective electrode method or an ion chromatography method, and the content of the fluorine element in each sample is calculated.
The utility model discloses a concrete example is applied to explain the principle and the implementation mode of the utility model, and the explanation of the above example is only used to help understand the method and the core idea of the utility model; meanwhile, for the general technical personnel in the field, according to the idea of the present invention, there are changes in the concrete implementation and the application scope. In summary, the content of the present specification should not be construed as a limitation of the present invention.
Claims (9)
1. A high-flux high-temperature hydrolysis device is characterized in that: the device comprises a multi-channel heating furnace, a combustion pipe, a sample placer, a sample injector, a water vapor generation control device, a carrier gas control device and a condensation receiving device, wherein the combustion pipe penetrates through the multi-channel heating furnace, the two ends of the combustion pipe are respectively an inlet end and an outlet end, the inlet end is provided with a plug, the sample injector is used for pushing the sample placer into the combustion pipe from the inlet end, the combustion pipe is provided with a first branch pipe and a second branch pipe, the first branch pipe is arranged on the combustion pipe close to the inlet end, the second branch pipe is arranged on the combustion pipe between the first branch pipe and the inlet end, each first branch pipe is connected with the water vapor generation control device, the water vapor generation control device is used for generating fractions and controlling the fraction flow entering each first branch pipe, each second branch pipe is connected with the carrier gas control device, the carrier gas control device is used for controlling the flow of carrier gas entering each second branch pipe, the condensation receiving device comprises a water-cooling machine, a plurality of condensation pipes and a plurality of receiving bottles, each condensation pipe comprises an inner pipe and an outer pipe fixedly sleeved outside the inner pipe, each outlet end is connected with an inlet of one inner pipe, an outlet of each inner pipe is introduced into one receiving bottle, and the outer pipe is communicated with the water-cooling machine to circularly cool fractions in the inner pipes.
2. The high-flux high-temperature hydrolysis apparatus according to claim 1, wherein: the water vapor generation control device comprises a temperature control electric furnace, a water vapor generation bottle and a multi-way switch joint, wherein the temperature control electric furnace is used for heating water in the water vapor generation bottle and controlling the temperature of the water in the water vapor generation bottle, an inlet pipe of the multi-way switch joint is connected with the water vapor generation bottle, outlet pipes of the multi-way switch joint are connected with the first branch pipes, and control switches are arranged on the outlet pipes of the multi-way switch joint.
3. The high-flux high-temperature hydrolysis apparatus according to claim 1, wherein: the carrier gas control device comprises a carrier gas bottle and a flow control valve, wherein the inlet of the flow control valve is connected with the outlet of the carrier gas bottle, and the outlet of the flow control valve is connected with the second branch pipe.
4. The high-flux high-temperature hydrolysis apparatus according to claim 1, wherein: the combustion tube is a quartz combustion tube.
5. The high-flux high-temperature hydrolysis apparatus according to claim 1, wherein: the sample placer is a quartz boat.
6. The high-flux high-temperature hydrolysis apparatus according to claim 1, wherein: the sample injector is a nickel-chromium alloy sample injector.
7. The high-flux high-temperature hydrolysis apparatus according to claim 3, wherein: and a flow dividing device is arranged at an outlet of the flow control valve and uniformly divides the carrier gas to each second branch pipe.
8. The high-flux high-temperature hydrolysis apparatus according to claim 1, wherein: the condenser pipe is a spherical condenser pipe.
9. The high-flux high-temperature hydrolysis apparatus according to claim 1, wherein: and the outer pipes are connected in series and then communicated with the water cooler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920757792.5U CN210269334U (en) | 2019-05-24 | 2019-05-24 | High-flux high-temperature hydrolysis device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920757792.5U CN210269334U (en) | 2019-05-24 | 2019-05-24 | High-flux high-temperature hydrolysis device |
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| Publication Number | Publication Date |
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| CN210269334U true CN210269334U (en) | 2020-04-07 |
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| CN201920757792.5U Expired - Fee Related CN210269334U (en) | 2019-05-24 | 2019-05-24 | High-flux high-temperature hydrolysis device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111721609A (en) * | 2020-05-18 | 2020-09-29 | 包头稀土研究院 | Pretreatment device and method for simultaneously treating multiple samples of hydrothermal distillation fluorine |
| CN114062522A (en) * | 2020-07-30 | 2022-02-18 | 湖南三德盈泰环保科技有限公司 | Sample pretreatment automation device and method |
-
2019
- 2019-05-24 CN CN201920757792.5U patent/CN210269334U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111721609A (en) * | 2020-05-18 | 2020-09-29 | 包头稀土研究院 | Pretreatment device and method for simultaneously treating multiple samples of hydrothermal distillation fluorine |
| CN114062522A (en) * | 2020-07-30 | 2022-02-18 | 湖南三德盈泰环保科技有限公司 | Sample pretreatment automation device and method |
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