A sample gas extraction device for testing total sulfur and effective sulfur content of non-metallic powder

Abstract

The invention discloses a sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powder, and relates to the field of sulfur content testing instruments for non-metallic powder materials, including a furnace body with a furnace head installed on the top, a quartz sample tube installed in the furnace body, and the top of the quartz sample tube is sealed and connected to the furnace head through a sealing ring; a crucible support base is installed at the bottom of the furnace body, and the crucible support base is installed with a crucible support through a connecting piece, and the crucible support is used to hold samples; a lifting cylinder connected to the crucible support base is arranged below the furnace body; a top-blown oxygen path joint and a sample gas outlet connected to the quartz sample tube are respectively provided on the furnace head, and a detector is connected to the outer end of the sample gas outlet; a reflector is arranged on the inner wall of the furnace body, and an infrared heating tube is arranged between the reflector and the quartz sample tube. The invention has high temperature control accuracy, stable SO2 release rate, and can effectively improve the accuracy of sulfur analysis.

Description

Technical Field

[0001] The invention relates to the field of instruments for testing the sulfur content of non-metallic powder materials, in particular to a sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powders. Background Art

[0002] Sulfur is a common element in materials. Both metal and non-metal powders contain a certain amount of sulfur. Traditionally, sulfur detection has focused on the metal field, especially steel. Because sulfur mainly comes from raw materials for steelmaking (such as mineral powder, various furnace charges, etc.), it has a strong impact on the performance of steel. Excessive sulfur will make steel brittle. Therefore, it is very important to accurately test the sulfur content in raw material mineral powder and other powder furnace charges, which also puts forward higher requirements for sulfur measuring instruments.

[0003] After searching standards and patents, the current technology uses a resistance furnace or a high-frequency furnace to melt and extract the sample, so that the sulfur in the sample escapes and reacts with O2 to generate SO2, and then detects the SO2 content to measure it. However, both the resistance furnace and the high-frequency furnace have very obvious defects when measuring non-metallic mineral powders, which are as follows:

[0004] High frequency furnace: It has high melting efficiency for metal materials, but extremely low melting efficiency for powder materials such as non-metals and semiconductors, and the conversion rate is very unstable. The sampling volume is very small, usually less than 1g. However, for powder non-metal and mineral powder samples, the sampling volume should be 30-50g. The sampling of high frequency furnace is not representative, and the blank signal is affected. The stability of the analysis result is very poor, which is not suitable for measuring samples of mineral powder and solid non-metallic raw materials. High frequency furnace cannot achieve precise constant temperature, so it cannot be used to conduct kinetic studies on elements in different valence states. Ore powder sometimes needs to measure the S content in different forms (such as sulfur concentrate, which needs to measure the content of effective sulfur and total sulfur at the same time. The effective sulfur is set at 850℃ and the total sulfur is at 1260℃). High frequency furnace is only suitable for measuring total sulfur, but cannot be used for accurate determination of effective sulfur in mineral powder such as sulfur concentrate.

[0005] Resistance furnace: The temperature rises and falls very slowly. It takes 1.5-2 hours to preheat the machine and 2-3 hours to cool it down. The test efficiency is extremely low and the failure rate is very high. Summary of the invention

[0006] The purpose of the present invention is to provide a sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powders to solve the problems existing in the above-mentioned prior art. It has high temperature control accuracy, stable SO2 release rate, and can effectively improve the accuracy of sulfur analysis.

[0007] To achieve the above object, the present invention provides the following solutions:

[0008] The invention provides a sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powder, comprising a furnace body, a furnace head is installed on the top of the furnace body, and a groove is provided in the furnace head; a quartz sample tube is fixedly installed in the furnace body, and the top of the quartz sample tube is sealed and connected to the open end of the groove of the furnace head through a sealing ring; a crucible support base is installed at the bottom of the furnace body, and a groove is provided on the crucible support base, and a crucible support is installed in the groove of the crucible support base through a connecting piece, and the crucible support is used to contain samples; a lifting cylinder is arranged below the furnace body, and the lifting cylinder is connected to the crucible support base, and when the lifting cylinder drives the crucible support base to rise, the open end of the groove of the crucible support base can be sealed and connected to the bottom of the quartz sample tube through a sealing ring; a top-blown oxygen path joint and a sample gas outlet connected to the quartz sample tube are respectively provided on the furnace head, and a detector is connected to the outer end of the sample gas outlet; a reflector is arranged on the inner wall of the furnace body, and an infrared heating tube is arranged between the reflector and the quartz sample tube.

[0009] Optionally, a dust filter with a cylindrical structure and openings at both ends is provided in the groove of the furnace head, and a sieve-like mesh is provided on the side wall of the dust filter; the bottom of the dust filter is cooperatively connected with the top opening of the quartz sample tube; the sample gas outlet is connected with the quartz sample tube through the dust filter.

[0010] Optionally, a purge cylinder is installed above the furnace head, and the rotating rod of the purge cylinder passes through the furnace head and is connected to an internal hollow oxygen gun rod. An oxygen gun nozzle is opened at the bottom of the oxygen gun rod, and the oxygen gun nozzle is located above the crucible support; the top-blowing oxygen line joint is connected to the oxygen gun rod.

[0011] Optionally, a cleaning copper wire wheel brush and a cleaning steel wire wheel brush are sleeved on the oxygen gun rod, the cleaning copper wire wheel brush is located in the dust filter, and the cleaning steel wire wheel brush is located in the quartz sample tube; an ash discharge hole is opened on one side of the bottom of the groove of the crucible support base.

[0012] Optionally, a carrier gas inlet is provided on a connecting piece located in the groove of the crucible support base; when the lifting cylinder drives the crucible support base to rise, the carrier gas inlet can be connected to the inside of the quartz sample tube; and an oxygen carrier gas circuit connector connected to the carrier gas inlet is installed at the bottom of the crucible support base.

[0013] Optionally, a circulating water pipeline is embedded in the side wall of the furnace body, and the circulating water pipeline is respectively connected with a water inlet and a water outlet, and the water inlet and the water outlet are respectively opened on the outer wall of the furnace body.

[0014] Compared with the prior art, the present invention has achieved the following technical effects:

[0015] The furnace has high temperature control accuracy, which can improve the melting stability of samples (especially non-metallic samples). The release rate of SO2 is stable, which can effectively improve the accuracy of sulfur analysis. It has high efficiency and fast heating rate, which can reach more than 500℃ in 1 minute. The sample can be tested immediately after the machine is turned on without preheating time. Different temperature control modes can be controlled by software to control the release of sulfur at different temperatures. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0017] Figure 1 This is a schematic diagram of the structure of a sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powders of the present invention;

[0018] Explanation of the accompanying reference numerals: 1. furnace body, 2. quartz sample tube, 3. crucible support base, 4. crucible support, 5. lifting cylinder, 6. oxygen carrier gas line connector, 7. carrier gas inlet, 8. ash discharge hole, 9. furnace head, 10. dust filter, 11. top blowing oxygen line connector, 12. sample gas outlet, 13. cleaning cylinder, 14. oxygen gun rod, 15. oxygen gun nozzle, 16. cleaning wire wheel brush, 17. cleaning copper wire wheel brush, 18. water inlet, 19. water outlet, 20. infrared heating tube, 21. reflector. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] The purpose of the present invention is to provide a sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powders to solve the problems existing in the above-mentioned prior art. It has high temperature control accuracy, stable SO2 release rate, and can effectively improve the accuracy of sulfur analysis.

[0021] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0022] The present invention provides a sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powders, such as Figure 1As shown, it includes a furnace body 1 made of aluminum alloy, a furnace head 9 is installed on the top of the furnace body 1, and a groove is opened in the furnace head 9; a quartz sample tube 2 is fixedly installed in the furnace body 1, and the top of the quartz sample tube 2 is sealed and connected to the open end of the groove of the furnace head 9 through a sealing ring; a crucible support base 3 is installed at the bottom of the furnace body 1, and a groove is opened on the crucible support base 3, and a crucible support 4 is installed in the groove of the crucible support base 3 through a connecting piece, and the crucible support 4 is used to hold the sample; a lifting cylinder 5 is arranged below the furnace body 1, and the lifting cylinder 5 is connected to the crucible support base 3, and when the lifting cylinder 5 drives the crucible support base 3 to rise, the open end of the groove of the crucible support base 3 can be sealed and connected to the bottom of the quartz sample tube 2 through a sealing ring; a top-blown oxygen path connector 11 and a sample gas outlet 12 connected to the quartz sample tube 2 are respectively opened on the furnace head 9, and a detector is connected to the outer end of the sample gas outlet 12; a reflector 21 is arranged on the inner wall of the furnace body 1, and an infrared heating tube 20 is arranged between the reflector 21 and the quartz sample tube 2.

[0023] Further preferably, a dust filter 10 with a cylindrical structure and openings at both ends is arranged in the groove of the furnace head 9, and a sieve-like mesh with an aperture of 0.5um is opened on the side wall of the dust filter 10; the bottom of the dust filter 10 is connected with the top opening of the quartz sample tube 2; the sample gas outlet 12 is connected with the quartz sample tube 2 through the dust filter 10. A cleaning cylinder 13 is installed above the furnace head 9, and the rotating rod of the cleaning cylinder 13 passes through the furnace head 9 and is connected to the hollow oxygen gun rod 14 inside. The bottom of the oxygen gun rod 14 is provided with an oxygen gun nozzle 15, and the oxygen gun nozzle 15 is located above the crucible support 4; the top blowing oxygen line joint 11 is connected with the oxygen gun rod 14. A cleaning copper wire wheel brush 17 and a cleaning steel wire wheel brush 16 are sleeved on the oxygen gun rod 14, and the cleaning copper wire wheel brush 17 is located in the dust filter 10, and the cleaning steel wire wheel brush 16 is located in the quartz sample tube 2; an ash discharge hole 8 is opened on one side of the bottom of the groove of the crucible support base 3. A carrier gas inlet 7 is provided on the connector in the groove of the crucible support base 3; when the lifting cylinder 5 drives the crucible support base 3 to rise, the carrier gas inlet 7 can be connected to the inside of the quartz sample tube 2; an oxygen carrier gas line connector 6 connected to the carrier gas inlet 7 is installed at the bottom of the crucible support base 3. A circulating water pipeline is embedded in the side wall of the furnace body 1, and the circulating water pipeline is respectively connected to a water inlet 18 and a water outlet 19, and the water inlet 18 and the water outlet 19 are respectively opened on the outer wall of the furnace body 1.

[0024] Specifically, the quartz sample tube 2 is installed in the furnace body 1 and does not contact the inner wall of the furnace body 1. The lower end of the quartz sample tube 2 is covered with an O-type gas sealing ring. When the lifting cylinder 5 rises, the crucible support base 3 is driven to rise. The crucible support base 3 is in close contact and sealed with the O-ring at the lower end of the quartz sample tube. The upper end of the quartz sample tube 2 is connected to the lower end of the furnace head 9 and is sealed by the O-type sealing ring. There are two gas path connectors on the furnace head 9, namely the top blowing oxygen path connector 11 and the sample gas outlet 12 connector. During analysis, the sample gas is blocked by the dust filter 10 with a cylindrical sieve mesh structure, and then connected to the detector of the instrument through the sample gas outlet 12. At the end of the analysis, the back-blowing gas enters the furnace head through the sample gas outlet 12. , used to purge the dust filter 10, and the dust that falls down is discharged from the ash discharge hole 8 on the crucible support base 3. The dust filter 10 is installed in the furnace head 9, and is used to filter the dust generated when the sample is burned to prevent the dust from entering the detector from the sample gas outlet 12. During analysis, oxygen enters the oxygen gun rod 14 in the furnace head 9 and is sent to the oxygen gun nozzle 15 to blow oxygen into the ceramic crucible containing the sample. At the same time, oxygen enters from the oxygen carrier line connector 6 and then enters the quartz sample tube 2 from the carrier gas inlet 7 on the crucible support base 3 to ensure that the sample is fully burned. The generated sample gas is blocked by the dust filter 10 and then connected to the detector of the instrument from the sample gas outlet 12 for analysis and testing.

[0025] The upper end of the furnace head 9 is sealed and connected to the cleaning cylinder 13, the oxygen gun rod 14 is connected to the cleaning cylinder 13 and the oxygen gun nozzle 15, the cleaning wire wheel brush 16 and the cleaning copper wire wheel brush 17 are fixedly installed at the upper and lower ends of the oxygen gun rod 14, when the cleaning cylinder 13 is extended and retracted, the dust filter 10 and the quartz sample tube 2 are cleaned simultaneously, and the cleaning process is an independent process, which is carried out under non-weighing working conditions. During the cleaning process, the top blowing oxygen path connector 11 is misaligned with the air inlet of the oxygen gun rod 14, but ventilation is not required at this time and is not affected. The two are reset during work.

[0026] During analysis, a ceramic crucible containing a weighed sample is placed on a crucible holder 4. The crucible holder 4 is made of cylindrical ceramics. The crucible holder 4 is fixed on a crucible holder base 3. The crucible holder base 3 is connected to the shaft of a lifting cylinder 5. The lifting cylinder 5 rises so that the crucible holder base 3 contacts and seals with the sealing ring at the lower end of the quartz sample tube 2. At the same time, the sample is sent into the furnace. At this time, the top blowing oxygen line connector 11 and the oxygen carrier line connector 6 simultaneously blow oxygen into the sample chamber (combustion tube). The infrared heating tube 2 0 emits infrared light, which is reflected by the reflector 21 embedded in the furnace body 1 and focused on the sample in the quartz sample tube 2, so that the sample burns and releases sulfur dioxide, which comes out from the sample gas outlet and is connected to the detector through the air pipe. At the same time, the water inlet 18 and the water outlet 19 arranged on the furnace body 1 are connected to the external water circulation machine for circulation, so as to cool the furnace body 1. After the analysis is completed, the cleaning cylinder 13 drives the two wheel brushes to clean the quartz sample tube 2 and the dust filter 10, and the dust is discharged from the ash discharge hole 8.

[0027] The present invention adopts an infrared focusing furnace to make the sample heat up and fully melt. The sulfur therein reacts with the carrier gas O2 in the sample tube to generate SO2, and the sulfur content is measured by the infrared detector of the instrument. The infrared focusing furnace can meet the maximum 20g sample detection and is suitable for various powders and solid non-metallic raw materials. The furnace temperature is set and accurately controlled by the software program. It can instantly rise to the set temperature during heating, and the temperature control accuracy can reach 0.1°C. Therefore, it is very convenient to realize a variety of temperature control modes such as step, linear, or stable temperature, which is very meaningful for studying the release degree of sulfur at different temperatures. The working efficiency is very high, no preheating is required, and an external water circulation machine is connected to achieve efficient heat dissipation of the furnace body to avoid high temperature damage to the furnace body and scalding. At the same time, it can also make the furnace body cool quickly and shorten the shutdown cooling time. The water discharged after heat dissipation can also be used for water-heating heaters, and the cold end water can be reused for cooling the infrared focusing furnace, which is energy-saving and environmentally friendly.

[0028] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powder, characterized in that: The invention comprises a furnace body, a furnace head is installed on the top of the furnace body, and a groove is provided in the furnace head; a quartz sample tube is fixedly installed in the furnace body, and the top of the quartz sample tube is sealed and connected to the open end of the groove of the furnace head through a sealing ring; a crucible support base is installed at the bottom of the furnace body, and a groove is provided on the crucible support base, and a crucible support is installed in the groove of the crucible support base through a connecting piece, and the crucible support is used to hold samples; a lifting cylinder is arranged under the furnace body, and the lifting cylinder is connected to the crucible support base, and when the lifting cylinder drives the crucible support base to rise, the open end of the groove of the crucible support base can be sealed and connected to the bottom of the quartz sample tube through a sealing ring; a top-blown oxygen path connector and a sample gas outlet connected to the quartz sample tube are respectively provided on the furnace head, and a detector is connected to the outer end of the sample gas outlet; the furnace body A reflecting mirror is arranged on the inner wall, and an infrared heating tube is arranged between the reflecting mirror and the quartz sample tube; a cleaning cylinder is installed above the furnace head, and the rotating rod of the cleaning cylinder passes through the furnace head and is connected to an internal hollow oxygen gun rod, and an oxygen gun nozzle is provided at the bottom of the oxygen gun rod, and the oxygen gun nozzle is located above the crucible support; the top-blowing oxygen path joint is connected to the oxygen gun rod; a carrier gas inlet is provided on the connecting piece located in the groove of the crucible support base; when the lifting cylinder drives the crucible support base to rise, the carrier gas inlet can be connected to the inside of the quartz sample tube; an oxygen carrier gas path joint connected to the carrier gas inlet is installed at the bottom of the crucible support base; a circulating water pipeline is embedded in the side wall of the furnace body, and the circulating water pipeline is respectively connected with a water inlet and a water outlet, and the water inlet and the water outlet are respectively opened on the outer wall of the furnace body.

2. The sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powder according to claim 1, characterized in that: A dust filter with a cylindrical structure and openings at both ends is arranged in the groove of the furnace head, and a sieve-like mesh is opened on the side wall of the dust filter; the bottom of the dust filter is matched and connected with the top opening of the quartz sample tube; the sample gas outlet is connected with the quartz sample tube through the dust filter.

3. The sample gas extraction device for testing the total sulfur and effective sulfur content of non-metallic powder according to claim 2, characterized in that: The oxygen gun rod is sleeved with a cleaning copper wire wheel brush and a cleaning steel wire wheel brush, the cleaning copper wire wheel brush is located in the dust filter, and the cleaning steel wire wheel brush is located in the quartz sample tube; an ash discharge hole is opened on one side of the bottom of the groove of the crucible support base.

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