CN110849765A - Oil sample pollution-free carbonization instrument and application thereof - Google Patents
Oil sample pollution-free carbonization instrument and application thereof Download PDFInfo
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Abstract
The invention relates to an oil sample pollution-free carbonization instrument and application thereof, relating to the field of chemical analysis instruments, comprising a carbonization chamber, wherein the top end of the carbonization chamber is connected with a first conduit which is connected with the output end of a nitrogen output device through a first two-way electromagnetic valve, the bottom end of the carbonization chamber is communicated with the top end of an oil receiver through a second conduit, the carbonization chamber also comprises an oxidation chamber, the top end of the oxidation chamber is respectively communicated with a third conduit and a fourth conduit, the other end of the third conduit is connected with a first port of a three-way electromagnetic valve, a second port of the three-way electromagnetic valve is connected with the output end of an oxygen input device through a fifth conduit, the fifth conduit is also communicated with a humidifier through a second two-way electromagnetic valve, a third port of the three-way electromagnetic valve is communicated with the first conduit through a sixth conduit, the other end of the fourth conduit is communicated with a second conduit, and the bottom end of the oxidation chamber is; the invention realizes the purpose of pollution-free carbonization of the oil sample and realizes self-cleaning of the carbonization chamber.
Description
Technical Field
The invention relates to a chemical analysis instrument, in particular to an instrument for carrying out carbonization analysis on an oil sample and application thereof.
Background
The carbon residue value of an oil product refers to the mass percentage of carbon residues formed after the oil product is subjected to evaporation and thermal cracking under a specific high-temperature condition. The main substances forming carbon residue in petroleum products are colloids, asphaltenes and polycyclic aromatic hydrocarbons. Generally, the carbon residue value increases when the amount of unstable hydrocarbons and colloids in the oil product is large or the amount of sulfur, oxygen and nitrogen compounds is large, so that the carbon residue is an indirect index of the content of colloidal substances, polycyclic aromatic hydrocarbons and unstable compounds in the oil product. The carbon residue of 10% residue of diesel fuel is a function of distillation range and degree of refining, and the lighter the fraction of diesel fuel, the better the refining, and the lower the carbon residue value. The lubricating oil made of heavy oil containing more jelly has higher carbon residue value, and the refining depth of the lubricating oil can be indirectly seen through the carbon residue value. Therefore, the determination of the carbon residue value of petroleum products has great significance for production and application.
At present, the carbon residue determination method mainly comprises three methods, namely a Kongshi method (GB/T268), an electric furnace method (SH/T170) and a micro method (GB/T17144). The Kangshi method is a standard method commonly adopted by all countries in the world, the micro method is a simple, convenient and efficient carbon residue determination method commonly adopted at home and abroad in recent years, and China is formally listed as a national standard method in 1997; the electric furnace method is from the original Soviet Union. The conradson method for measuring carbon residue has other disadvantages besides requiring the operator to be skilled in heating temperature and time: firstly, only one sample can be tested at a time, and the process of measuring the sample is slow; secondly, the measurement accuracy is low, and even the measurement results of experienced personnel are not easy to repeat and even can deviate greatly; thirdly, more samples are needed; more importantly, since the fume hood cannot be opened during the experiment, the air quality of the measuring chamber is seriously affected by the poisonous substances generated by the high-temperature distillation and the decomposition products. The defects of the electric furnace method are similar to those of the Kangshi method carbon residue, the electric furnace method carbon residue has the advantages that a plurality of samples can be tested at one time, the data repeatability is better than that of the Kangshi method carbon residue, and the efficiency is equivalent to that of the micro-method carbon residue. The micro-method carbon residue has the advantages of the Kangshi method, can overcome the defects of the electric furnace method, is increasingly widely applied in recent years, has good repeatability and high automation degree, but in the process of determining the micro-method carbon residue, the allowable sampling quantity is small, the lower limit of detection is higher, meanwhile, the air pressure in the coke oven is greater than the environment, so that the surface stain of an instrument is serious, and the carbon black in the coke oven is obvious after the coke oven is used for a period of time, so that on one hand, a sealing cover generates a gap, on the other hand, the circulation of oil gas is blocked, and part of the oil gas is directly emptied to pollute the environment.
The invention not only has the characteristic of micro-method carbon residue, but also can be operated by one key; meanwhile, the allowable sampling amount is large, and the lower limit of detection is low; the sample chamber is carbonized in the atmosphere of micro negative pressure and nitrogen, and the surface of the instrument is free of stains; the sample chamber has the self-cleaning function without obvious carbon black, the sealing is not tight, and the front side of the sealing door is opened/closed more conveniently than the upper opening/closing of a sealing cover of micro-method carbon residue; one part of the oil gas is condensed and collected, and the other part of the oil gas is purified through oxidation, so that a large amount of toxic and harmful substances are prevented from being exhausted; the sample chamber has the devices and procedures of safe leakage, small nitrogen pressure, no start, electronic door lock, over-temperature power off and the like.
Documents closely related to the present invention:
⑴ CN 202075195 U. an automatic micro carbon residue tester for petroleum products, when the tester is used, nitrogen is firstly filled in a constant temperature bathtub, then the constant temperature bathtub is heated to 500 ℃ for 15 minutes, then the temperature is reduced to below 200 ℃, a test tube is taken out and weighed, the measured data, namely the micro carbon residue, is the percentage of the residual quantity of the test tube to the original weight of the test sample, and the invention is not mentioned in the aspect of waste gas purification and whether the whole system is ensured to be under the anaerobic condition.
⑵ CN207586150U the invention provides an automatic micro carbon residue tester which can meet the requirements of national standard on temperature rise rate and constant temperature precision, and has the advantages of long heating life, simple processing technology and convenient assembly and replacement.
⑶ CN202329126U A high-temperature furnace device suitable for petroleum carbon residue tester emphasizes on the heating mode of the furnace, and solves the problem that the heater in the embedded furnace wall is difficult to disassemble and repair after being damaged.
⑷ CN206930545U is a device for measuring the carbon residue of materials, which relates to a device for measuring the carbon residue of materials and solves the problems of low temperature control and oxygen insulation degree of the existing carbon residue device.
⑸ model of deny, the research on the correlation of the carbon residue determination method and data, petroleum refining and chemical industry 2005,36(10):61-65, the text compares 3 methods of Conradson method (GB/T268), electric furnace method (SH/T170) and micro method (GB/T17144) for determining the carbon residue of petroleum products, obtains the correlation and exceptional condition analysis of data comparability, and evaluates the advantages and disadvantages of the 3 methods.
Disclosure of Invention
The invention mainly solves the technical problem of providing an oil sample pollution-free carbonizer and application thereof, so as to solve the technical problem that the operating environment is polluted in the oil sample carbonization analysis process in the prior art.
The invention provides an oil sample pollution-free carbonization instrument, which comprises a carbonization chamber with a cavity inside and a heating function, wherein the top end of the carbonization chamber is connected with a first conduit, the other end of the first conduit is connected with one end of a first two-way electromagnetic valve, the other end of the first two-way electromagnetic valve is connected with the output end of a nitrogen output device, the bottom end of the carbonization chamber is communicated with the top end of an oil receiver through a second conduit, the oil sample pollution-free carbonization instrument also comprises an oxidation chamber with a cavity inside and a heating function, the top end of the oxidation chamber is respectively communicated with a third conduit and a fourth conduit, the other end of the third conduit is connected with a first port of a three-way electromagnetic valve, a second port of the three-way electromagnetic valve is connected with the output end of an oxygen input device through a fifth conduit, the fifth conduit is also communicated with a humidifier through a second two-way electromagnetic valve, a third port of the three-way electromagnetic valve is communicated with the first conduit through a, the other end of the fourth conduit is communicated with the second conduit, the bottom end of the oxidation chamber is connected with the input end of the negative pressure generator through a seventh conduit, the inner wall of the carbonization chamber is made of a stainless steel body, and a movable reticular stainless steel supporting plate is arranged at the bottom of the stainless steel body.
Further, install first temperature sensor and pressure sensor in the carbonization chamber, install second temperature sensor in the oxidation chamber, still be provided with the controller, carbonization chamber, first two solenoid valve, nitrogen gas output device, oxidation chamber, three-way solenoid valve, oxygen input device, second two solenoid valve, humidifier, negative pressure generator, first temperature sensor, pressure sensor, second temperature sensor are respectively with controller signal connection.
Furthermore, movable mounting has the closed door on the preceding terminal surface of carbonization room, install the electromagnetic lock on the closed door, the electromagnetic lock with controller signal connection.
Further, a liquid level sensor is installed in the oil receiver and is in signal connection with the controller.
Further, a noble metal oxide catalyst is also arranged in the oxidation chamber.
Further, an air inlet channel is arranged in the vertical wall at the top of the carbonization chamber, at least ten air inlets for communicating the air inlet channel with the inner cavity of the carbonization chamber are uniformly formed in the inner wall of the carbonization chamber corresponding to the air inlet channel, and the air inlet channel is communicated with the first conduit.
Furthermore, an alarm is further arranged and is in signal connection with the controller.
Further, the pressure sensor is a micro negative pressure sensor.
The invention also provides a method for carrying out pollution-free carbonization on the oil sample by using the oil sample pollution-free carbonization instrument, which comprises the following steps:
all units of the equipment are in a closed state in the initial state
Step 1, after a quartz or porcelain vessel containing an oil sample is placed in a carbonization chamber, a sealing door is closed and an electromagnetic lock is controlled to be locked through a controller;
and 2, controlling equipment through a controller to perform the following operations:
A. starting a negative pressure generator to enable each conduit, the carbonization chamber and the oxidation chamber to keep a negative pressure state;
B. opening a nitrogen output device and a first two-way electromagnetic valve, enabling nitrogen to enter a gas inlet channel through a first guide pipe, enabling the nitrogen to uniformly flow into a carbonization chamber from top to bottom after being dispersed through an air inlet, taking away other gases in the carbonization chamber, and finally discharging the gases after sequentially passing through a second guide pipe, a fourth guide pipe, an oxidation chamber, a seventh guide pipe and a negative pressure generator, and finally enabling the carbonization chamber to be filled with the nitrogen;
C. opening the oxygen input device, the three-way electromagnetic valve and the oxidation chamber, enabling oxygen to enter the oxidation chamber through the fifth conduit and the third conduit in sequence, and finally to be discharged after finally passing through the seventh conduit and the negative pressure generator, and enabling the oxidation chamber to start a heating function;
D. starting a first temperature sensor, a pressure sensor, a second temperature sensor and a liquid level sensor;
E. the controller adjusts the rotating speed of the negative pressure generator and the nitrogen output speed of the nitrogen output device through the data detected by the pressure sensor, so that the negative pressure value detected by the pressure sensor is within-15 Pa to-50 Pa;
F. the controller controls the heating function of the oxidation chamber to be turned on or off through the second temperature sensor, so that the temperature detected by the second temperature sensor is within the range of 500-550 ℃;
the steps A to F are carried out synchronously;
When the step F is finished, the controller controls the carbonization chamber to start the heating function, the first temperature sensor monitors the internal temperature, when the temperature reaches 500-;
After step 3 is finished, the carbonization chamber, the oxygen input device and the oxidation chamber are closed simultaneously through the controller, the carbonization chamber is cooled in the environment of nitrogen input until the temperature data in the carbonization chamber detected by the first temperature sensor is lower than 60 ℃, the electromagnetic lock is opened, the sealing door is opened to take out and weigh the quartz or porcelain vessel, the residual carbon analysis is carried out, then the sealing door is closed and the electromagnetic lock is controlled to be locked through the controller, and then the following steps are carried out:
G. self-cleaning
The nitrogen output device, the first two-way electromagnetic valve and the oxidation chamber are controlled to be closed through the controller, the heating function of the carbonization chamber is started, the first temperature sensor monitors the temperature inside the carbonization chamber, when the temperature reaches 500-550 ℃, the controller feeds back and adjusts the carbonization chamber through the first temperature sensor to maintain the temperature inside the carbonization chamber at 500-550 ℃, the oxygen input device and the humidifier are started, the three-way electromagnetic valve is adjusted, water vapor generated by the humidifier is mixed with oxygen in the fifth conduit, then the water vapor is guided into the first conduit through the three-way electromagnetic valve by using the sixth conduit and enters the carbonization chamber through the air inlet channel and the air inlet hole, carbon black in the carbonization chamber is subjected to chemical reaction with water vapor under the high-temperature action to generate carbon monoxide and hydrogen, and finally the carbon monoxide and the hydrogen are discharged finally after sequentially passing through the second conduit, the fourth conduit, the oxidation chamber, the seventh conduit and the negative;
H. the duration of the step G is 10-15 min;
and 5, after the step 4 is finished, the equipment stops running.
Further, when the temperature data detected by the first temperature sensor is more than 600 ℃/the temperature data detected by the second temperature sensor is more than 700 ℃, the controller starts an alarm and enables the carbonization chamber/oxidation chamber to be powered off and stop running.
Compared with the prior art, the invention has the following advantages:
the oxidation chamber is communicated with the carbonization chamber, and the negative pressure generator is used for maintaining the negative pressure state of the equipment, so that the product of high-temperature distillation and decomposition of the oil sample enters the oxidation chamber under the drive of nitrogen to be mixed with oxygen and then oxidized, the defect that the product is directly discharged into a measurement environment is avoided, and the air quality of the measurement environment is improved; in the whole carbonization analysis process, the discharged gas is only carbon dioxide and water, so that the aim of zero emission and no pollution is fulfilled; after carbonization is finished, water vapor is led into the carbonization chamber to react with carbon black in the carbonization chamber at high temperature to generate carbon monoxide and hydrogen, so that the defect of carbon deposition blackening of the carbonization chamber is avoided, the cleanness of the carbonization chamber is kept, and the problems that the carbon black possibly blocks an air inlet and blocks oil gas discharge are avoided; the equipment is simple to operate.
Drawings
FIG. 1 is a schematic view showing the structure of an oil sample non-contamination carbonizer in example 1;
in the figure: 1. a carbonization chamber; 2. a first conduit; 3. a first two-way solenoid valve; 4. a nitrogen output device; 5. a second conduit; 6. an oil receiver; 7. an oxidation chamber; 8. a third conduit; 9. a fourth conduit; 10. a three-way electromagnetic valve; 11. a fifth conduit; 12. an oxygen input device; 13. a second two-way solenoid valve; 14. a humidifier; 15. a sixth conduit; 16. a seventh conduit; 17. a negative pressure generator; 18. a pressure sensor; 19. a first temperature sensor; 20. a second temperature sensor; 21. a closing door; 22. an electromagnetic lock; 23. a liquid level sensor; 24. an intake passage.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Referring to fig. 1, in the present embodiment, there is provided an oil sample non-pollution carbonization apparatus, comprising a carbonization chamber 1 with a hollow interior and a heating function, a first conduit 2 connected to a top end of the carbonization chamber 1, the other end of the first conduit 2 connected to one end of a first two-way solenoid valve 3, the other end of the first two-way solenoid valve 3 connected to an output end of a nitrogen output device 4, a bottom end of the carbonization chamber 1 communicated with a top end of an oil receiver 6 through a second conduit 5, an oxidation chamber 7 with a hollow interior and a heating function, a top end of the oxidation chamber 7 respectively communicated with a third conduit 8 and a fourth conduit 9, the other end of the third conduit 8 connected to a first port of a three-way solenoid valve 10, a second port of the three-way solenoid valve 10 connected to an output end of an oxygen input device 12 through a fifth conduit 11, the fifth conduit 11 further connected to a humidifier 14 through a second two-way solenoid valve 13, the third port of the three-way electromagnetic valve 10 is communicated with the first conduit 2 through a sixth conduit 15, the other end of the fourth conduit 9 is communicated with the second conduit 5, the bottom end of the oxidation chamber 7 is connected with the input end of a negative pressure generator 17 through a seventh conduit 16, the inner wall of the carbonization chamber 1 is made of a stainless steel body, and the bottom of the stainless steel body is provided with a movable reticular stainless steel supporting disk.
In this embodiment, in order to facilitate control of the device and realize automatic operation, the following settings are also performed:
the carbonization chamber 1 is internally provided with a first temperature sensor 19 and a pressure sensor 18 for detecting the internal temperature and the air pressure, the oxidation chamber 7 is internally provided with a second temperature sensor 20 for detecting the internal temperature, and the carbonization chamber is further provided with a controller 22, wherein the carbonization chamber 1, the first two-way electromagnetic valve 3, the nitrogen output device 4, the oxidation chamber 7, the three-way electromagnetic valve 10, the oxygen input device 12, the second two-way electromagnetic valve 13, the humidifier 14, the negative pressure generator 17, the first temperature sensor 19, the pressure sensor 18 and the second temperature sensor 20 are respectively in signal connection with the controller 22.
In this embodiment, in order to facilitate placing the oil sample, the following settings are also made:
the front end surface of the carbonization chamber 1 is movably provided with a closing door 21, the closing door 21 is provided with an electromagnetic lock 22, and the electromagnetic lock 22 is in signal connection with a controller 22.
In this embodiment, in order to prevent the waste liquid in the oil receiver 6 from overflowing, a liquid level sensor 23 is installed in the oil receiver 6, and the liquid level sensor 23 is in signal connection with the controller 22.
In this embodiment, in order to accelerate the oxidation reaction in the oxidation chamber 7, a noble metal oxide catalyst is further disposed in the oxidation chamber 7 to accelerate the oil gas oxidation process.
In the embodiment, in order to realize that the gas can uniformly enter the carbonization chamber 1 from top to bottom, in the embodiment, an air inlet channel 24 is arranged in a vertical wall at the top of the carbonization chamber 1, at least ten air inlet holes for communicating the air inlet channel 24 with the inner cavity of the carbonization chamber 1 are uniformly formed in the inner wall of the carbonization chamber 1 corresponding to the air inlet channel 24, and the air inlet channel 24 is communicated with the first conduit 2;
in this embodiment, in order to avoid accidents, an alarm is further provided, and the alarm is in signal connection with the controller 22.
In the present embodiment, the pressure sensor 18 is a micro-negative pressure sensor.
In the embodiment, all temperature sensors are platinum-rhodium thermocouple type high-temperature-resistant corundum tube temperature sensors with the model of WRP-130, in the embodiment, the pressure sensors are Panasonic DP-102-HT digital display pressure sensors, the controller is a Siemens programmable controller PLC CPU224, a touch screen is a Kunlun Tong TPC1062K, in the embodiment, all two-way electromagnetic valves are 2W-160-15, in the embodiment, the three-way electromagnetic valve is a three-way electromagnetic valve with the model of VA7010-25, and in the embodiment, a liquid level sensor with the model of MIK-P260 is selected; in this embodiment, the negative pressure generator is specifically configured with a double-layer gas injection pipe.
Example 2
This example provides a method for the contamination-free carbonization of oil samples using the apparatus described in example 1, comprising the steps of:
all units of the equipment are in a closed state in the initial state
Step 1, after a quartz or porcelain vessel containing an oil sample is placed in a carbonization chamber 1, a sealing door 21 is closed, and an electromagnetic lock 22 is controlled to be locked by a controller 22;
step 2, controlling the device to perform the following operations by the controller 22:
A. starting the negative pressure generator 17 to keep the negative pressure state in each conduit, the carbonization chamber 1 and the oxidation chamber 7;
B. opening a nitrogen output device 4 and a first two-way electromagnetic valve 3, enabling nitrogen to enter an air inlet channel 24 through a first conduit 2, enabling the nitrogen to uniformly flow into a carbonization chamber 1 from top to bottom after being dispersed through an air inlet, taking away other gases in the carbonization chamber 1, and finally discharging the gases after sequentially passing through a second conduit 5, a fourth conduit 9, an oxidation chamber 7, a seventh conduit 16 and a negative pressure generator 17, and finally enabling the carbonization chamber 1 to be filled with the nitrogen;
C. opening an oxygen input device 12, a three-way electromagnetic valve 10 and an oxidation chamber 7, enabling oxygen to enter the oxidation chamber 7 through a fifth conduit 11 and a third conduit 8 in sequence and finally to be discharged after finally passing through a seventh conduit 16 and a negative pressure generator 17, and enabling the oxidation chamber 7 to start a heating function;
D. turning on the first temperature sensor 19, the pressure sensor 18, the second temperature sensor 20 and the level sensor 23;
E. the controller 22 adjusts the rotating speed of the negative pressure generator 17 and the nitrogen output speed of the nitrogen output device 4 through the data detected by the pressure sensor 18, so that the negative pressure value detected by the pressure sensor 18 is within-15 Pa to-50 Pa;
F. the controller 22 controls the heating function of the oxidation chamber 7 to be turned on or off through the second temperature sensor 20, so that the temperature detected by the second temperature sensor 20 is within the range of 500-550 ℃;
the steps A to F are carried out synchronously;
When the step F is finished, the controller 22 controls the carbonization chamber 1 to start the heating function, the first temperature sensor 19 monitors the internal temperature, when the temperature reaches 500-;
After step 3 is completed, the controller 22 is used for simultaneously closing the carbonization chamber 1, the oxygen input device 12 and the oxidation chamber 7, the carbonization chamber 1 is cooled in the environment of nitrogen input until the temperature data detected by the first temperature sensor 19 is lower than 60 ℃, the electromagnetic lock 22 is opened, the closing door 21 is opened, the quartz or porcelain vessel is taken out and weighed, the residual carbon analysis is carried out, then the closing door 21 is closed, the electromagnetic lock 22 is controlled to be locked through the controller 22, and then the following steps are carried out:
G. the nitrogen output device 4, the first two-way electromagnetic valve 3 and the oxidation chamber 7 are controlled to be closed by the controller 22, the heating function of the carbonization chamber 1 is started, the temperature in the carbonization chamber 1 is monitored by the first temperature sensor 19, when the temperature reaches 500 plus 550 ℃, the controller 22 feeds back and adjusts the carbonization chamber 1 by the first temperature sensor 19 to maintain the temperature in the carbonization chamber 1 at 500 plus 550 ℃, the oxygen input device 12 and the humidifier 14 are started, the three-way electromagnetic valve 10 is adjusted, the water vapor generated by the humidifier 14 is mixed with the oxygen in the fifth conduit 11, then is guided into the first conduit 2 by the three-way electromagnetic valve 10 through the sixth conduit 15 and enters the carbonization chamber 1 through the air inlet channel 24 and the air inlet, the carbon black in the carbonization chamber 1 is subjected to chemical reaction with the water vapor under the action of high temperature to generate carbon monoxide and hydrogen, and finally, the carbon monoxide and the hydrogen are sequentially led into the second conduit 5, the fourth conduit 9, the seventh conduit 16 and the negative pressure generator 17 are finally discharged;
H. the duration of the step G is 10-15 min;
and 5, after the step 4 is finished, the equipment stops running.
In the present embodiment, when the first temperature sensor 19 detects temperature data greater than 600 deg.C/the second temperature sensor 20 detects temperature data greater than 700 deg.C, the controller 22 activates the alarm and causes the carbonization/oxidation chambers 1, 7 to be powered off and stopped.
EXAMPLE 3
In this example, 12.4133g of oil A was weighed out and subjected to the procedure of example 2, to obtain 0.0187g of residual substance. The carbon residue value of oil A is calculated to be 0.15%.
Example 4
In this example, 2.2365g of oil B was weighed out and subjected to the procedure of example 2, to obtain 0.1021g of residual substance. The carbon residue value of oil B is calculated to be 4.56%.
Example 5
In this example, 1.0331g of oil C was weighed out and subjected to the procedure of example 2 to obtain 0.2019g of residual substance. The carbon residue value of oil C is calculated to be 19.54%.
Example 6
In this example, 30.0126g of oil D was weighed out and subjected to the procedure of example 2, to obtain 0.0072g of the remaining material. The carbon residue value of oil D is calculated to be 0.024%.
Finally, it should also be noted that the above-mentioned list is only a specific embodiment of the invention. It is clear that the invention is not limited to the above examples, but that there are many applications that require oil/viscous organic carbon residue determination. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (10)
1. A pollution-free oil sample carbonizer comprises a carbonization chamber with a cavity inside and a heating function, and is characterized in that the top end of the carbonization chamber is connected with a first conduit, the other end of the first conduit is connected with one end of a first two-way electromagnetic valve, the other end of the first two-way electromagnetic valve is connected with the output end of a nitrogen output device, the bottom end of the carbonization chamber is communicated with the top end of an oil receiver through a second conduit, the oil sample carbonizer also comprises an oxidation chamber with a cavity inside and a heating function, the top end of the oxidation chamber is respectively communicated with a third conduit and a fourth conduit, the other end of the third conduit is connected with a first port of a three-way electromagnetic valve, a second port of the three-way electromagnetic valve is connected with the output end of an oxygen input device through a fifth conduit, the fifth conduit is also communicated with a humidifier through a second two-way electromagnetic valve, and a third port of the three-way electromagnetic valve is communicated with the first conduit through a sixth conduit, the other end of the fourth conduit is communicated with the second conduit, the bottom end of the oxidation chamber is connected with the input end of the negative pressure generator through a seventh conduit, the inner wall of the carbonization chamber is made of a stainless steel body, and a movable reticular stainless steel supporting plate is arranged at the bottom of the stainless steel body.
2. The oil sample non-pollution carbonization instrument according to claim 1, wherein a first temperature sensor and a pressure sensor are installed in the carbonization chamber, a second temperature sensor is installed in the oxidation chamber, and a controller is further provided, wherein the carbonization chamber, the first two-way solenoid valve, the nitrogen output device, the oxidation chamber, the three-way solenoid valve, the oxygen input device, the second two-way solenoid valve, the humidifier, the negative pressure generator, the first temperature sensor, the pressure sensor and the second temperature sensor are respectively in signal connection with the controller.
3. The oil sample carbonization instrument without pollution according to claim 2, wherein a closing door is movably mounted on the front end surface of the carbonization chamber, and an electromagnetic lock is mounted on the closing door and is in signal connection with the controller.
4. The non-pollution carbonization instrument for oil samples according to claim 3, wherein a liquid level sensor is installed in the oil receiver, and the liquid level sensor is in signal connection with the controller.
5. The oil sample carbonization instrument without pollution according to claim 4, wherein a noble metal oxide catalyst is further disposed in the oxidation chamber.
6. The oil sample non-pollution carbonization instrument according to claim 5, wherein an air inlet channel is provided in the vertical wall at the top of the carbonization chamber, the inner wall of the carbonization chamber corresponding to the air inlet channel is uniformly provided with at least ten air inlets communicating the air inlet channel with the inner cavity of the carbonization chamber, and the air inlet channel is communicated with the first conduit.
7. The oil sample non-pollution carbonization instrument according to claim 6, wherein an alarm is further provided, and the alarm is in signal connection with the controller.
8. The oil sample carbonization instrument without pollution according to claim 7, wherein the pressure sensor is a micro negative pressure sensor.
9. A method for the non-contamination carbonization of an oil sample by using the non-contamination carbonization apparatus for an oil sample according to claim 8, comprising the steps of:
all units of the equipment are in a closed state in the initial state
Step 1, after a quartz or porcelain vessel containing an oil sample is placed in a carbonization chamber, a sealing door is closed and an electromagnetic lock is controlled to be locked through a controller;
and 2, controlling equipment through a controller to perform the following operations:
A. starting a negative pressure generator to enable each conduit, the carbonization chamber and the oxidation chamber to keep a negative pressure state;
B. opening a nitrogen output device and a first two-way electromagnetic valve, enabling nitrogen to enter a gas inlet channel through a first guide pipe, enabling the nitrogen to uniformly flow into a carbonization chamber from top to bottom after being dispersed through an air inlet, taking away other gases in the carbonization chamber, and finally discharging the gases after sequentially passing through a second guide pipe, a fourth guide pipe, an oxidation chamber, a seventh guide pipe and a negative pressure generator, and enabling the carbonization chamber to be filled with the nitrogen;
C. opening the oxygen input device, the three-way electromagnetic valve and the oxidation chamber, enabling oxygen to enter the oxidation chamber through the fifth conduit and the third conduit in sequence, and finally to be discharged after finally passing through the seventh conduit and the negative pressure generator, and enabling the oxidation chamber to start a heating function;
D. starting a first temperature sensor, a pressure sensor, a second temperature sensor and a liquid level sensor;
E. the controller adjusts the rotating speed of the negative pressure generator and the nitrogen output speed of the nitrogen output device through the data detected by the pressure sensor, so that the negative pressure value detected by the pressure sensor is within-15 Pa to-50 Pa;
F. the controller controls the heating function of the oxidation chamber to be turned on or off through the second temperature sensor, so that the temperature detected by the second temperature sensor is within the range of 500-550 ℃;
the steps A to F are carried out synchronously;
step 3, carbonization
When the step F is finished, the controller controls the carbonization chamber to start the heating function, the first temperature sensor monitors the internal temperature, when the temperature reaches 500-;
step 4, cooling and sampling
After step 3 is finished, the carbonization chamber, the oxygen input device and the oxidation chamber are closed simultaneously through the controller, the carbonization chamber is cooled in the environment of nitrogen input until the temperature data in the carbonization chamber detected by the first temperature sensor is lower than 60 ℃, the electromagnetic lock is opened, the sealing door is opened to take out and weigh the quartz or porcelain vessel, the residual carbon analysis is carried out, then the sealing door is closed and the electromagnetic lock is controlled to be locked through the controller, and then the following steps are carried out:
G. self-cleaning
The nitrogen output device, the first two-way electromagnetic valve and the oxidation chamber are controlled to be closed through the controller, the heating function of the carbonization chamber is started, the first temperature sensor monitors the temperature inside the carbonization chamber, when the temperature reaches 500-550 ℃, the controller feeds back and adjusts the carbonization chamber through the first temperature sensor to maintain the temperature inside the carbonization chamber at 500-550 ℃, the oxygen input device and the humidifier are started, the three-way electromagnetic valve is adjusted, water vapor generated by the humidifier is mixed with oxygen in the fifth conduit, then the water vapor is guided into the first conduit through the three-way electromagnetic valve by using the sixth conduit and enters the carbonization chamber through the air inlet channel and the air inlet hole, carbon black in the carbonization chamber is subjected to chemical reaction with water vapor under the high-temperature action to generate carbon monoxide and hydrogen, and finally the carbon monoxide and the hydrogen are discharged finally after sequentially passing through the second conduit, the fourth conduit, the oxidation chamber, the seventh conduit and the negative;
H. the duration of the step G is 10-15 min;
and 5, after the step 4 is finished, the equipment stops running.
10. A method according to claim 9, wherein the controller activates the alarm and de-energizes the carbonator/oxidizer chamber to stop operation when the first temperature sensor detects temperature data greater than 600 ℃/the second temperature sensor detects temperature data greater than 700 ℃.
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