CN219038580U - High-temperature hydrolysis device - Google Patents

High-temperature hydrolysis device Download PDF

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Publication number
CN219038580U
CN219038580U CN202222535201.4U CN202222535201U CN219038580U CN 219038580 U CN219038580 U CN 219038580U CN 202222535201 U CN202222535201 U CN 202222535201U CN 219038580 U CN219038580 U CN 219038580U
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furnace
temperature
condenser
boat
tube
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CN202222535201.4U
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徐金龙
叶金燕
刘建芳
李展江
杨树洁
林海
唐斌
曲强
李春雄
谭智毅
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Zhanjiang Customs Technical Center
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Zhanjiang Customs Technical Center
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Abstract

The application relates to the field of detection, especially relates to a high temperature hydrolysis device, and the device includes: vapor generator, high temperature furnace, boiler tube, condenser and absorption volumetric flask, wherein: the steam output end of the steam generator is connected with the air inlet of the furnace tube; the high temperature furnace is provided with 3 or more furnace chambers, and heating devices are respectively arranged in the furnace chambers, so that the key temperature in the hydrolysis process can be controlled conveniently; the furnace tube is arranged in the high-temperature furnace, the sample introduction boat and the push rod are arranged in the furnace tube, the sample introduction boat is connected with the push rod, and when the push rod pushes the sample introduction boat to move, the sample introduction boat is switched to different furnace chambers, so that the sample can be controlled to undergo hydrolysis processes at different temperatures more reliably, and the accuracy of sample detection is improved.

Description

High-temperature hydrolysis device
Technical Field
The utility model belongs to the field of detection, and particularly relates to a high-temperature hydrolysis device.
Background
To detect the fluorine and chlorine content of asphalt (including diluted asphalt), it is necessary to hydrolyze the asphalt at high temperatures to detect the chlorine and fluorine content of the asphalt. At present, a high-temperature hydrolysis mode is generally adopted, an asphalt sample is placed in a high-temperature furnace, and after the asphalt sample is subjected to high-temperature hydrolysis, water vapor for high-temperature hydrolysis is absorbed by an absorption liquid to measure chlorine content and fluorine content.
The current high-temperature hydrolysis device hydrolyzes through a high-temperature furnace, and generally adjusts the temperature of the high-temperature furnace, so that a detection sample can be subjected to high-temperature hydrolysis through heating at different temperatures. The temperature control of the high-temperature furnace of the device is troublesome, and the key temperature control in the hydrolysis process of the asphalt sample is inconvenient, so that the detection precision is not improved.
Disclosure of Invention
The utility model aims to provide a high-temperature hydrolysis device, which solves the problems that the temperature control of the high-temperature hydrolysis device in the prior art is troublesome, the key temperature control in the hydrolysis process of an asphalt sample is inconvenient and the detection precision is not easy to improve by adopting the design of continuous and different furnace chambers.
In a first aspect, embodiments of the present application provide a high temperature hydrolysis apparatus, the high temperature hydrolysis apparatus includes a steam generator, a high temperature furnace, a furnace tube, a condenser, and an absorption volumetric flask, wherein:
the steam output end of the steam generator is connected with the air inlet of the furnace tube;
the high-temperature furnace is provided with 3 or more furnace chambers, and heating devices are respectively arranged in the furnace chambers;
the furnace tube is arranged in the high-temperature furnace, a sample introduction boat and a push rod are arranged in the furnace tube, the sample introduction boat is connected with the push rod, and when the push rod pushes the sample introduction boat to move, the sample introduction boat is switched to different furnace chambers;
the first end of the condenser is connected with the air outlet of the furnace tube, and the second end of the condenser is connected with the input port of the absorption volumetric flask.
With reference to the first aspect, in a first possible implementation manner of the first aspect, the furnace tube is further provided with an oxygen input port for inputting oxygen, and a drain port for draining water, and the oxygen input port and the drain port are disposed on an air inlet side of the furnace tube.
With reference to the first possible implementation manner of the first aspect, in a second possible implementation manner of the first aspect, a first flowmeter is provided at the oxygen inlet, and/or a second flowmeter is provided at the gas inlet of the furnace tube.
With reference to the first aspect, in a third possible implementation manner of the first aspect, the condenser includes a condensation pipe and a condensation cavity, the condensation pipe is disposed in the condensation cavity, the condensation cavity includes a condensate water inlet and a condensate water outlet, the condensate water inlet is located at the second end of the condenser, and the condensate water outlet is located at the first end of the condenser.
With reference to the third possible implementation manner of the first aspect, in a fourth possible implementation manner of the first aspect, the condensation duct is spiral or folded.
With reference to the first aspect, in a fifth possible implementation manner of the first aspect, a fixed pool is further disposed in the furnace tube, the sample boat is disposed in the fixed pool, and the sample boat is connected to the push rod through the fixed pool.
With reference to the first aspect, in a sixth possible implementation manner of the first aspect, the high-temperature furnace includes 3 furnace chambers, and a direction from the air inlet to the air outlet, and a temperature of the furnace chambers is 300 degrees celsius, 600 degrees celsius, and 900 degrees celsius in sequence.
With reference to the sixth possible implementation manner of the first aspect, in a seventh possible implementation manner of the first aspect, a thermocouple and a temperature sensor are respectively disposed in a furnace chamber of the high temperature furnace, and the thermocouple heats the furnace chamber through a temperature signal detected by the temperature sensor.
With reference to the first aspect, in an eighth possible implementation manner of the first aspect, the absorption volumetric flask includes a first volumetric flask and a second volumetric flask, the first volumetric flask is connected in series with the second volumetric flask, and an alkaline solution for collecting hydrolysis results is disposed in the first volumetric flask and the second volumetric flask.
With reference to the first aspect, in a ninth possible implementation manner of the first aspect, the steam generator includes an electric furnace and a round-bottomed flask, the round-bottomed flask is disposed in the electric furnace, and a moving wheel is disposed at a bottom of the electric furnace.
In the utility model, the temperature in the furnace chamber can be controlled more reliably by arranging 3 or more furnace chambers in the high-temperature furnace and arranging the heating devices in the furnace chambers respectively. The furnace tube is arranged in the high-temperature furnace, the sample introduction boat in the furnace tube is moved by the push rod, so that the sample introduction boat is switched to different furnace chambers in the furnace tube, the position of the sample introduction boat in the furnace chamber can be controlled more accurately and reliably, the hydrolysis process of samples at different temperatures can be controlled more reliably, and the accuracy of sample detection is improved.
Drawings
Fig. 1 is a schematic diagram of a high-temperature hydrolysis apparatus according to an embodiment of the present utility model.
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present utility model more apparent, the present utility model will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the utility model.
Fig. 1 is a schematic structural diagram of a hydrolysis apparatus according to an embodiment of the present utility model. As shown in fig. 1, the high-temperature hydrolysis apparatus includes: a steam generator 101, a high temperature furnace 102, furnace tubes 103, a condenser 104 and an absorption capacity bottle 105, wherein:
the steam output end of the steam generator 101 is connected with the air inlet of the furnace tube 103.
The high temperature furnace 102 is provided with 3 or more furnace chambers 1021, and heating devices 1022 are respectively arranged in the furnace chambers 1021;
the furnace tube 103 is disposed in the high temperature furnace 102, a sample boat 1031 and a push rod 1032 are disposed in the furnace tube 102, the sample boat 1031 is connected with the push rod 1032, and when the push rod 1032 pushes the sample boat 1031 to move, the sample boat 1031 is switched to a different furnace chamber 1021.
The first end of the condenser 104 is connected with the air outlet of the furnace tube 103, and the second end of the condenser 104 is connected with the input port of the absorption volumetric flask 105.
Wherein the water vapor generator 101 is for generating water vapor. The water vapor generator 101 may include a round bottom flask 1011 and an electric furnace 1012. Round-bottom flask 1011 is mounted on electric furnace 1012 and round-bottom flask 1011 may be heated by electric furnace 1012 to boil water in round-bottom flask to produce water vapor.
In order to facilitate the movement of the steam generator 101, a moving wheel 1013 may be provided at the bottom of the electric furnace 1012, and the position of the steam generator 101 may be conveniently adjusted by the rotation of the moving wheel 1013.
To facilitate flow control of the steam, a second flow meter may be provided between the steam generator 101 and the furnace tube, such as at the inlet of the furnace tube. The rate of pyrolysis is controlled by adjusting and counting the steam generated by steam generator 101 and entering furnace tubes 103 based on the second flow meter.
To facilitate movement of the steam generator 101, a hose may be included between the steam generator 101 and the furnace tube 103 to reduce the impact on the furnace tube 103 when the steam generator 101 is repositioned.
The high temperature furnace 102 is provided with 3 or more than 3 furnace chambers 1021 therein, and each furnace chamber is provided with a heating device 1022 therein. In a possible implementation, the furnace chambers 1021 are sequentially arranged, and the furnace chambers may be round and isolated from each other. The temperature in the cavity is 300 degrees celsius, 600 degrees celsius and 900 degrees celsius in order from the air inlet connected with the steam generator 101 to the air outlet connected with the condenser 104. The temperature inside the cavity 1021 may be detected by a temperature sensor, and the heating device 1022 is controlled to perform heating based on the detected temperature, so that the temperature inside the cavity 102 is maintained constant. The heating device 1022 may include a thermocouple or the like.
Furnace tube 103 may be made of quartz and may have a temperature resistance value greater than 1200 degrees celsius. The furnace tube 103 may extend through each furnace chamber 1021 of the high temperature furnace 102. A sample boat 1031 and a push rod 1032 may be provided in the furnace 103. The sample boat 1031 may be directly or indirectly coupled to the push rod 1032. Pushing the sample boat 1031 by the push rod 1032 can switch the sample boat to a different chamber 1021 position.
In a possible implementation, the furnace 103 further includes a fixed pool 1033, where the fixed pool 1033 is used for placing the sample boat 1031, and the push rod 1032 may be connected to the fixed pool 1033, and the position of the fixed pool 1033 in the furnace 103 is changed by the push rod 1032, so that the sample boat 1031 is switched to a different furnace chamber 1021. The fixed pool 1033 may fix the sample boat 1031 such that the sample boat 1031 can stably move within the furnace tube 103.
In a possible implementation, the push rod 1032 is also provided with graduations. When a worker pushes the sample boat or the fixed pool by using the push rod 1032, the position of the sample boat 1031 or the fixed pool 1033 in the furnace tube 103 can be known through the scale, so that the sample boat or the fixed pool is convenient to accurately position.
An oxygen inlet and a water outlet can be further arranged at the air inlet of the furnace tube 103, and oxygen is introduced through the oxygen inlet, so that the generation efficiency of the high-temperature hydrolysis reaction can be effectively promoted. The drain opening is provided at a low level of the furnace tube 103, for example, may be provided at a bottom of the furnace tube 103 or the like. And the liquid water generated in the furnace tube is discharged through the water outlet.
In order to control the oxygen input amount conveniently, a first flowmeter is further arranged at the oxygen input port of the furnace tube 103, and the input oxygen amount is determined through the first flowmeter, so that the reaction process of high-temperature hydrolysis can be controlled more accurately.
The condenser 104 is used for condensing the high-temperature hydrolyzed water vapor. The first end of the condenser 104 is connected with the air outlet of the furnace tube 103, and the second end of the condenser 104 is connected with the input port of the absorption volumetric flask 105.
The condenser 104 includes a condensation chamber 1041 and a condensation pipe 1042, wherein the condensation chamber 1041 is provided with a condensed water inlet and a condensed water outlet, the condensed water inlet is disposed at the second end of the condenser 104, and the condensed water outlet is disposed at the first end of the condenser 104, so as to facilitate effective condensation treatment of water vapor.
The condensation pipe 1042 may be in a spiral shape, a zigzag shape or other curved shapes, so as to increase the contact area between the condensation pipe 1042 and the condensed water and improve the condensation effect.
The absorption flask 105 is used to absorb a high-temperature thermal specimen. The absorption capacity bottle 105 may include one or two or more. When there are two or more absorption vials 105, the hydrolyzed sample may be sufficiently absorbed by the series. When the sample hydrolyzed at high temperature is asphalt, and the data measured by hydrolysis at high temperature is chlorine content or fluorine content, sodium hydroxide solution or sodium bicarbonate solution may be set in the absorption capacity bottle 105. The connecting pipe connected with the air outlet of the condenser 104 is arranged below the liquid level of the absorption alkali liquid, and the chlorine and fluorine in the hydrolysis sample are absorbed by the alkali liquid.
After the high-temperature hydrolysis device is assembled, the measurement operation of high-temperature hydrolysis can be performed according to the following method:
1. 0.50g + -0.01 g or 5mL of an analytical test sample (asphalt sample) is weighed by a pipette and placed in a sample boat 1031 for high temperature hydrolysis.
2. 10mL of sodium hydroxide solution or sodium bicarbonate solution is removed and placed in an absorption liquid volumetric flask 105, the absorption liquid volumetric flask 105 is placed at the lower end of the connecting pipe of the condenser tube 1042 and the connecting pipe of the condenser tube 1042 is placed below the level of the absorption liquid. Under the condition of introducing oxygen and steam, the sample injection push rod is taken down, a sample injection boat containing diluted asphalt is placed into the furnace tube 103, and the push rod 1032 is inserted to plug the silica gel plug. The front end of the sample introduction boat 1031 (porcelain boat) is pushed to a pre-measured area of about 300 ℃ for 5min, then pushed to an area of about 600 ℃ for 5min, then pushed to a constant temperature area of 900 ℃, the sample introduction push rod is retracted, and the sample is continuously combusted and hydrolyzed in the constant temperature area for 15min.
During the whole operation, the evaporation capacity of the steam generator 101 is regulated, the absorption liquid is collected in the absorption liquid volumetric flask 105 for about 3 mL/min within 15min at the beginning of hydrolysis, and is collected for about 2.5 mL/min after 15min, and finally the total volume is controlled within 90 mL. Taking down the volumetric flask, diluting with water to a scale, shaking, filtering with a 0.22 μm filter membrane to obtain solution to be analyzed, detecting by ion chromatograph, and determining fluorine and chlorine content.
The foregoing description of the preferred embodiments of the utility model is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the utility model.

Claims (10)

1. The high-temperature hydrolysis device is characterized by comprising a water vapor generator, a high-temperature furnace, a furnace tube, a condenser and an absorption volumetric flask, wherein:
the steam output end of the steam generator is connected with the air inlet of the furnace tube;
the high-temperature furnace is provided with 3 or more furnace chambers, and heating devices are respectively arranged in the furnace chambers;
the furnace tube is arranged in the high-temperature furnace, a sample introduction boat and a push rod are arranged in the furnace tube, the sample introduction boat is connected with the push rod, and when the push rod pushes the sample introduction boat to move, the sample introduction boat is switched to different furnace chambers;
the first end of the condenser is connected with the air outlet of the furnace tube, and the second end of the condenser is connected with the input port of the absorption volumetric flask.
2. The apparatus according to claim 1, wherein the furnace tube is further provided with an oxygen input port for inputting oxygen, and a drain port for draining water, the oxygen input port and the drain port being provided on an inlet side of the furnace tube.
3. The high-temperature hydrolysis apparatus according to claim 2, wherein a first flowmeter is provided at the oxygen inlet port, and/or a second flowmeter is provided at the gas inlet port of the furnace tube.
4. The apparatus of claim 1, wherein the condenser comprises a condenser tube and a condenser chamber, the condenser tube is disposed in the condenser chamber, the condenser chamber comprises a condensate water inlet and a condensate water outlet, the condensate water inlet is located at the second end of the condenser, and the condensate water outlet is located at the first end of the condenser.
5. The apparatus according to claim 4, wherein the condenser tube is spiral or folded.
6. The high-temperature hydrolysis device according to claim 1, wherein a fixed pool is further arranged in the furnace tube, the sample boat is arranged in the fixed pool, and the sample boat is connected with the push rod through the fixed pool.
7. The high temperature hydrolysis apparatus according to claim 1, wherein the high temperature furnace comprises 3 furnace chambers, and the temperatures of the furnace chambers are 300 degrees celsius, 600 degrees celsius, and 900 degrees celsius in order from the air inlet to the air outlet.
8. The high-temperature hydrolysis apparatus according to claim 7, wherein a thermocouple and a temperature sensor are respectively provided in a cavity of the high-temperature furnace, and the thermocouple heats the cavity by a temperature signal detected by the temperature sensor.
9. The high-temperature hydrolysis apparatus according to claim 1, wherein the absorption volumetric flask comprises a first volumetric flask and a second volumetric flask, the first volumetric flask being connected in series with the second volumetric flask, and an alkaline solution for collecting hydrolysis results being provided in the first volumetric flask and the second volumetric flask.
10. The apparatus according to claim 1, wherein the steam generator comprises an electric furnace and a round bottom flask, and the bottom of the electric furnace is provided with a moving wheel.
CN202222535201.4U 2022-09-22 2022-09-22 High-temperature hydrolysis device Active CN219038580U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202222535201.4U CN219038580U (en) 2022-09-22 2022-09-22 High-temperature hydrolysis device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202222535201.4U CN219038580U (en) 2022-09-22 2022-09-22 High-temperature hydrolysis device

Publications (1)

Publication Number Publication Date
CN219038580U true CN219038580U (en) 2023-05-16

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202222535201.4U Active CN219038580U (en) 2022-09-22 2022-09-22 High-temperature hydrolysis device

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