A large-scale fluidized boiling chlorination furnace high temperature hearth online sampling device and method

Abstract

The present invention provides an online sampling device and method for a high-temperature furnace bed of a large-scale fluidized chlorination furnace. The sampling device comprises: a sampling port arranged on the boiling chlorination furnace, the sampling port is connected with a sampling pipeline, a sampler is connected at the other end of the sampling pipeline, the sampler is also connected with a negative extraction pipeline, a nitrogen pipeline and a sample outlet pipeline, and a sampling valve group, a negative extraction valve group, a nitrogen valve group and a sample outlet valve group are respectively arranged on the sampling pipeline, the negative extraction pipeline, the nitrogen pipeline and the sample outlet pipeline, respectively, for controlling the on-off of the sampling pipeline, the negative extraction pipeline, the nitrogen pipeline and the sample outlet pipeline. The present invention realizes online sampling outside the chlorination furnace through the arrangement of the above-mentioned sampling device. At the same time, the arrangement of the nitrogen pipeline avoids the blockage of the sample in the sampling pipeline. The negative extraction pipeline closes and collects the chlorine and / or titanium tetrachloride gas overflowed by the sampling at the same time, so as to avoid the gas escaping into the surrounding environment, thereby ensuring the health of the operator.

Description

Technical Field

[0001] The invention relates to the technical field of material sampling technology for a chemical fluidized reactor, and in particular to an online sampling device and method for a high-temperature furnace bed of a large fluidized boiling chlorination furnace. Background Art

[0002] The boiling chlorination method is a process in which titanium tetrachloride is produced by chlorination reaction at high temperature (900-1000°C) using chlorine as fluid and chlorinating agent, and a mixture of titanium raw material (rutile or high-titanium slag) and petroleum coke is suspended in a boiling furnace. It has the advantages of high production efficiency, low environmental pollution, and high degree of automation. With these advantages, the boiling chlorination method has become the mainstream method for producing crude titanium tetrachloride in the world.

[0003] The boiling chlorination process of titanium raw materials belongs to carbon addition chlorination. Carbon addition chlorination reaction is an exothermic reaction. The heat released by the reaction itself can make the chlorination reaction of titanium raw materials continue. The fixed carbon in petroleum coke can be converted into carbon monoxide or carbon dioxide in the boiling chlorination reaction. The ratio of titanium raw materials to petroleum coke (carbon ratio) can theoretically be calculated according to the content of each component in the titanium raw materials and the chlorination reaction equation, and can fluctuate within a wide range. However, the boiling chlorination reaction in actual production is far from reaching a state of equilibrium. The fluctuation range of the ratio of CO:CO2 generated by the reaction at the operating temperature is relatively large. If the carbon ratio is too low, the reaction cannot be fully carried out. If the carbon ratio is too high, it will not only increase the consumption of petroleum coke and the amount of slag, but also increase the gas, reduce the partial pressure of titanium tetrachloride in the gas phase, and is not conducive to the condensation of titanium tetrachloride.

[0004] Due to the different grades of titanium raw materials and high impurity content, impurities represented by calcium and magnesium chlorides will continue to increase and enrich in the bed during the chlorination process. These two chlorides have the characteristics of low melting point and high boiling point: the melting point of CaCl2 is 772℃, and the boiling point is greater than 1600℃; the melting point of MgCl2 is 714℃, and the boiling point is 1412℃. At a higher chlorination temperature (800-1000℃), it is in a molten state and is easy to stay in the fluidized bed. It is low in volatility and difficult to effectively remove. When the CaCl2 and MgCl2 of the fluidized layer material are enriched to a certain extent, the material begins to granulate or agglomerate, and the effective boiling space of the chlorination furnace is reduced, resulting in an increase in the pressure in the furnace, an increase in the pressure drop of the bed, difficulty in passing chlorine, violent fluctuations in the bed, difficulty in slagging, and a significant reduction in the chlorination rate. The boiling chlorination reaction cannot proceed normally, and the chlorine content of the tail gas increases, until the fluidized state is destroyed. According to relevant literature records, when the calcium and magnesium content in the bed of the chlorination furnace is greater than 3%, it is easy to cause bed compaction and fluidization destruction. Properly increasing the carbon ratio in the mixture is one of the effective methods to dilute the concentration of CaCl2 and MgCl2 in the bed. In addition to diluting the concentration of CaCl2 and MgCl2, the excess carbon in the reaction also plays a role in wrapping and isolating the particles of calcium and magnesium chlorides, preventing the particles from sticking to each other and growing into agglomerates, and avoiding bed compaction. However, an excessively large carbon ratio will affect the reaction diffusion process, reduce the chlorination rate, and cause waste, and accelerate the growth rate of bed pressure drop, increase the frequency of slag discharge, and reduce production capacity.

[0005] Therefore, there is an urgent need for an online sampling device suitable for the high-temperature furnace bed of a large fluidized boiling chlorination furnace. During the operation of the boiling chlorination furnace, the bed layer can be sampled online to check the carbon ratio and impurity content of the bed layer, and the mixing material feeding speed can be adjusted in time or the impurity content of the bed layer can be reduced by slag discharge, so as to effectively control the optimal fluidization reaction state in the furnace and ensure that the boiling chlorination reaction is carried out efficiently and smoothly.

[0006] Chinese patent CN201620774271.7 discloses a chlorination furnace sampling device, including a chlorination furnace body, a pipe connected to the inner cavity of the chlorination furnace body and capable of placing or removing a sampler, a control valve disposed on the upper portion of the pipe, and a nitrogen pipe disposed below the control valve. The patent samples by placing a sampler into the chlorination furnace. On the one hand, the temperature in the furnace is extremely high, and its operating device and sampler are easily damaged. On the other hand, when the sampler is placed in the pipe and taken out of the pipe, the pipe is in an unsealed state, and the overflow of harmful gases such as chlorine and / or titanium tetrachloride in the chlorination furnace cannot be prevented. At the same time, some harmful gases will also exist in the sampler, which is easy to cause damage to the health of the operator. Summary of the invention

[0007] The problem solved by the present invention is that, in the prior art, a chlorination furnace sampling device usually needs to place a sampler in the chlorination furnace for sampling. On the one hand, the sampler has a large loss. On the other hand, when the sampler is placed in and taken out, chlorine and / or titanium tetrachloride are prone to leakage. At the same time, some harmful gases may also exist in the sample, causing damage to the health of operators.

[0008] The invention discloses an online sampling device for a high-temperature furnace bed of a large-scale fluidized boiling chlorination furnace, which is used for online sampling of the boiling chlorination furnace and comprises: a sampling port arranged on the boiling chlorination furnace, the sampling port being arranged corresponding to the boiling section of the boiling chlorination furnace, the sampling port being connected with a sampling pipeline, the other end of the sampling pipeline being connected with a sampler, the sampler being further connected with a negative pressure extraction pipeline, a nitrogen pipeline and a sample outlet pipeline, the negative pressure extraction pipeline being used for extracting negative pressure, the nitrogen pipeline being used for conveying nitrogen into the sampler, the sample outlet pipeline being used for exporting a sample taken out from the sampler, and a sampling valve group, a negative pressure extraction valve group, a nitrogen valve group and a sample outlet valve group being respectively arranged on the sampling pipeline, the negative pressure extraction pipeline, the nitrogen pipeline and the sample outlet pipeline, and being respectively used for controlling the on-off of the sampling pipeline, the negative pressure extraction pipeline, the nitrogen pipeline and the sample outlet pipeline.

[0009] Through the above arrangement, when sampling is needed, first connect the sample outlet pipeline to release the material in the sampler, then connect the nitrogen pipeline to blow nitrogen into the sampler to purge the sampler to avoid residual samples in the sampler, then close the sample outlet pipeline and the nitrogen pipeline to prepare for sampling. When sampling, first connect the nitrogen pipeline to blow nitrogen into the sampler, and then connect the sampling pipeline to maintain the input of nitrogen to purge the sampling pipeline to ensure the smooth flow of the sampling pipeline, and then increase the flow of nitrogen to purge the sampling pipeline while agitating the material at the sampling port, and then close the nitrogen pipeline and connect. The negative pressure pipeline is drained to drain the sampler. At this time, the high-temperature material in the boiling chlorination furnace flows into the sampler under the action of the pressure difference between the inside and outside of the furnace body. After the sampling is completed, the sampling pipeline and the negative pressure pipeline are closed, and the sample outlet pipeline is connected to take out the high-temperature material in the sampler. After the high-temperature material is taken out, the nitrogen pipeline is connected to purge the sampler with nitrogen to ensure that the material therein is completely released. Then the sample outlet pipeline and the nitrogen pipeline are closed to end the sampling. At this time, the nitrogen pipeline is connected first, and then the sampling pipeline is connected. The sampling pipeline is purged with nitrogen to keep the sampling pipeline unobstructed to complete a sampling cycle.

[0010] Furthermore, a movable sampling bucket is provided at the outlet end of the sample outlet pipeline, and the sampling bucket is used to hold the sample taken out by the sampling device.

[0011] Not much material is taken out during one sampling process, which is not conducive to accurately obtaining information about the situation in the furnace, and the results of a single sampling may have large deviations. Sufficient samples can be taken out through multiple samplings, and after being evenly mixed in the sampling barrel, the samples are allowed to cool down naturally and then sent for inspection, which can effectively ensure the reliability of the sampling test results.

[0012] Furthermore, the sampling pipeline is made of Incone material.

[0013] The sampling pipeline made of Incone material is resistant to high temperature, material friction and chlorine corrosion, which can ensure the service life of the sampling pipeline in the environment of high temperature resistant materials, chlorine and titanium tetrachloride, and can realize repeated sampling of the chlorination furnace, ensuring the normal use of the sampling device.

[0014] Furthermore, the sampling valve group includes at least a first high-temperature ball valve and a second high-temperature ball valve, the negative pressure extraction valve group includes at least a first carbon steel ball valve, the nitrogen valve group includes at least a second carbon steel ball valve, and the sample outlet valve group includes at least a third high-temperature ball valve.

[0015] The sampling valve group is used to control the on-off of the sampling pipeline, and the sampling valve group is used to control the on-off of the sampling pipeline. Both need to be in direct contact with the high-temperature material taken out of the boiling chlorination furnace. The use of high-temperature ball valves can ensure their effectiveness. The negative extraction valve group is used to control the on-off of the negative extraction pipeline, and the nitrogen valve group is used to control the on-off of the nitrogen pipeline. Both do not need to be in direct contact with the high-temperature material. The use requirements can be met by using carbon steel ball valves to avoid cost waste.

[0016] Furthermore, a nitrogen flow meter and a pressure gauge are also provided on the nitrogen pipeline.

[0017] The nitrogen flow meter is used to control the flow of nitrogen, and the pressure gauge is used to detect the pressure of nitrogen, so as to complete the purging of the sampler, the purging of the sampling pipeline, and the agitation of the material at the sampling port.

[0018] Furthermore, the nitrogen flow meter is equipped with a magnetic filter, a check valve and a needle valve.

[0019] The magnetic filter is used to ensure the purity of nitrogen to avoid contamination of samples. The check valve and needle valve are used to prevent high-temperature gas and materials from flowing into the nitrogen pipeline, and are also used to assist in regulating the nitrogen flow rate.

[0020] The present invention also discloses a high-temperature furnace bed online sampling method, which is used for the online sampling device as described above, and comprises the following steps:

[0021] Step S1: Check that the sampling valve group, the negative extraction valve group, the nitrogen valve group, and the sample outlet valve group are all in a closed state;

[0022] Step S2: connecting the sample outlet pipeline to release the material in the sampler;

[0023] Step S3: connecting a nitrogen pipeline, inputting nitrogen into the sampler at a first preset pressure and a first preset flow rate, and purging the sampler;

[0024] Step S4: After the purge is completed, close the sample outlet pipeline and the nitrogen pipeline;

[0025] Step S5: connecting the nitrogen pipeline and the sampling pipeline in sequence, delivering nitrogen at a first preset pressure and a first preset flow rate, so that the nitrogen purges the sampling pipeline to keep it unobstructed;

[0026] Step S6: adjusting the nitrogen valve group to deliver nitrogen at a second preset pressure and a second preset flow rate to blow the material at the sampling port, and closing the nitrogen pipeline after maintaining the nitrogen gas for a first preset time;

[0027] Step S7: connecting the negative pressure extraction pipeline to perform negative pressure extraction and depressurization on the sampler, and the high-temperature material in the boiling chlorination furnace flows into the sampler through the sampling pipeline under the action of the pressure difference between the inside and outside of the furnace body;

[0028] Step S8: After the negative pressure is released for a second preset time, the negative pressure pipeline and the sampling pipeline are closed;

[0029] Step S9: connecting the sample outlet pipeline to guide the sample taken out from the sampler into the sampling bucket;

[0030] Step S10: connecting a nitrogen pipeline, inputting nitrogen into the sampler at a first preset pressure and a first preset flow rate, and purging the sampler to ensure that the sample is completely released;

[0031] Step S11: connecting the nitrogen pipeline and the sampling pipeline in sequence, delivering nitrogen at a first preset pressure and a first preset flow rate, so that the nitrogen purges the sampling pipeline to keep it unobstructed.

[0032] Through the above steps, the online sampling of the boiling chlorination furnace can be realized to check the carbon ratio and impurity content of the bed, timely adjust the feeding speed of the mixed material, or reduce the impurity content of the bed by means of slagging, so as to effectively control the optimal fluidized reaction state in the furnace, ensure that the boiling chlorination reaction is carried out efficiently and smoothly, and at the same time, balance the material addition, improve the chlorine utilization efficiency, and reduce the cost loss caused by excessive addition of raw materials. In addition, the high-temperature material is extracted through the negative extraction pipeline, and the closed sampling is completed. There is no risk of chlorine and titanium tetrachloride gas leakage during sampling and setting out, which ensures the personal health of the operator and is environmentally friendly.

[0033] Furthermore, when the boiling chlorination furnace is not started, steps S1-S4 are preparatory work before starting, and after step S4 is completed, the boiling chlorination furnace is started, and then steps S5-S11 are performed to take samples.

[0034] When the boiling chlorination furnace is not started, the sampler should be cleaned first to avoid residual materials in the sampler from contaminating the sampling sample.

[0035] Furthermore, when multiple samplings are required, after the first sampling step S11 is completed, steps S5 to S11 are repeatedly executed.

[0036] This setting can enable the sampling device to take samples multiple times in a short period of time, and then mix the samples taken multiple times together for testing, which can improve the accuracy of the test results and avoid the situation where the deviation of a single sampling is too large.

[0037] Furthermore, the first preset pressure is above 0.4 MPa, and the first preset flow rate is 5-10 m 3 / h, the second preset pressure is 0.4-0.6MPa, and the second preset flow rate is 15-20m 3 / h, the first preset time is 8-12 seconds, and the second preset time is 3-5 seconds.

[0038] By setting the above preset values, the purging of the sampler, the purging of the sampling pipeline, the agitation of the high-temperature material at the material taking port and the sampling of the high-temperature material are realized, and the online sampling work of the boiling chlorination furnace is completed. The bed carbon ratio and the impurity content can be checked, the feeding speed of the mixture can be adjusted in time, or the impurity content of the bed can be reduced by means of slag discharge, so as to effectively control the optimal fluidized reaction state in the furnace, ensure the boiling chlorination reaction to be carried out efficiently and smoothly, and at the same time, balance the material addition, improve the utilization efficiency of chlorine, and reduce the cost loss caused by excessive addition of raw materials.

[0039] Compared with the prior art, the large-scale fluidized boiling chlorination furnace high temperature hearth online sampling device and method of the present invention has the following advantages:

[0040] The present invention provides a sampling port in the boiling section of the chlorination furnace, and provides a sampling pipeline connected to the sampling port, the other end of the sampling pipeline is connected to a sampler, and the sampler is also connected to a negative extraction pipeline, a nitrogen pipeline and a sample outlet pipeline, so as to realize online sampling outside the chlorination furnace. At the same time, the setting of the nitrogen pipeline avoids the blockage of the sample in the sampling pipeline, and the negative extraction pipeline closes and collects the chlorine and / or titanium tetrachloride gas overflowed at the same time during sampling, so as to avoid the gas from escaping into the surrounding environment, thereby ensuring the health of the operator. At the same time, the sampling device provided by the present invention can realize multiple sampling in a short time, which is conducive to the real-time monitoring of the reaction state in the chlorination furnace, and ensures that the reaction in the boiling chlorination furnace is carried out efficiently and smoothly. The sampling device provided by the present invention is simple and convenient to operate, the sampling process is carried out in a closed manner, and there is no risk of leakage of chlorine and titanium tetrachloride gas during sampling and placing, thereby avoiding the risk of causing damage to the health of the operator. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 It is a structural schematic diagram of the high-temperature furnace bed online sampling device of a large-scale fluidized boiling chlorination furnace according to an embodiment of the present invention.

[0042] Description of reference numerals:

[0043] 1. Boiling chlorination furnace; 2. First high-temperature ball valve; 3. Second high-temperature ball valve; 4. Sampler; 5. First carbon steel ball valve; 6. Negative extraction pipeline; 7. Third high-temperature ball valve; 8. Second carbon steel ball valve; 9. Nitrogen flowmeter; 10. Pressure gauge; 11. Sampling barrel; 12. Sampling port; 13. Sampling pipeline; 14. Sample outlet pipeline; 15. Nitrogen pipeline. DETAILED DESCRIPTION

[0044] To make the purpose, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. The specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. It should be noted that the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict.

[0045] The following is a detailed description of an online sampling device and method for a high-temperature furnace bed of a large-scale fluidized boiling chlorination furnace according to an embodiment of the present invention in conjunction with the accompanying drawings.

[0046] Example 1

[0047] This embodiment provides a large-scale fluidized boiling chlorination furnace high temperature furnace bed online sampling device, such as Figure 1As shown, the online sampling for the boiling chlorination furnace 1 includes: a sampling port 12 arranged on the boiling chlorination furnace 1, the sampling port 12 is arranged corresponding to the boiling section of the boiling chlorination furnace 1, the sampling port 12 is connected to a sampling pipeline 13, the other end of the sampling pipeline 13 is connected to a sampler 4, the sampler 4 is also connected to a negative pressure extraction pipeline 6, a nitrogen pipeline 15 and a sample outlet pipeline 14, the negative pressure extraction pipeline 6 is used to extract negative pressure, the nitrogen pipeline 15 is used to transport nitrogen to the sampler 4, the sample outlet pipeline 14 is used to lead out the sample taken out from the sampler 4, and the sampling pipeline 13, the negative pressure extraction pipeline 6, the nitrogen pipeline 15 and the sample outlet pipeline 14 are respectively provided with a sampling valve group, a negative pressure extraction valve group, a nitrogen valve group and a sample outlet valve group, which are respectively used to control the on-off of the sampling pipeline 13, the negative pressure extraction pipeline 6, the nitrogen pipeline 15 and the sample outlet pipeline 14. Through the above arrangement, when sampling is required, the sample outlet pipeline 14 is first connected to release the material in the sampler 4, and then the nitrogen pipeline 15 is connected to blow nitrogen into the sampler 4 to purge the sampler 4 to avoid residual sample in the sampler 4, and then the sample outlet pipeline 14 and the nitrogen pipeline 15 are closed to prepare for sampling. When sampling, the nitrogen pipeline 15 is first connected to blow nitrogen into the sampler 4, and then the sampling pipeline 13 is connected to keep the input of nitrogen to purge the sampler 4. The sampling pipeline 13 is purged to ensure the smooth flow of the sampling pipeline 13, and then the flow rate of nitrogen is increased to purge the sampling pipeline 13 while agitating the material in the sampling port 12, and then the nitrogen pipeline is closed, the negative extraction pipeline 6 is connected, and the sampler 4 is negatively depressurized. At this time, the high-temperature material in the boiling chlorination furnace 1 flows into the sampler 4 under the action of the pressure difference between the inside and outside of the furnace body. After the sampling is completed, the sampling pipeline 13 and the negative extraction pipeline 6 are closed, and the sample outlet pipeline 14 is connected to release the high-temperature material in the sampler 4. The material is taken out. After the high-temperature material is taken out, the nitrogen pipeline 15 is connected, and the sampler 4 is purged with nitrogen to ensure that the material therein is completely released. Then the sample outlet pipeline 14 and the nitrogen pipeline 15 are closed to end the sampling. At this time, the nitrogen pipeline 15 is connected first, and then the sampling pipeline 13 is connected. The sampling pipeline 13 is purged with nitrogen to keep the sampling pipeline 13 unobstructed, and a sampling cycle is completed. During the sampling process, the chlorine gas and / or titanium tetrachloride gas in the boiling chlorination furnace 1 will be simultaneously discharged with the high-temperature material. Enter the sampler 4, but due to the existence of the negative extraction pipeline 6, the chlorine gas and / or titanium tetrachloride gas entering the sampler 4 will be extracted, avoiding the risk of them being discharged with the sample and causing damage to the health of the operator. At the same time, after the sampler 4 and the sampling pipeline 13 are purged with nitrogen, the sampling device can perform another sampling task in a short time, thereby realizing continuous monitoring of the high-temperature material in the boiling chlorination furnace 1, and helping to improve the operating stability in the boiling chlorination furnace 1.

[0048] As an optional embodiment, a movable sampling bucket 11 is provided at the outlet end of the sample outlet pipeline 14, and the sampling bucket 11 is used to hold the sample taken out by the sampling device. It should be understood that not much material is taken out in one sampling process, which is not conducive to accurately obtaining the situation information in the furnace, and the single sampling result may have a large deviation. Sufficient samples can be taken out through multiple samplings, and after being evenly mixed in the sampling bucket 11, the samples are allowed to cool naturally and then sent for inspection, which can effectively ensure the reliability of the sampling test results.

[0049] As an optional embodiment, the sampling pipeline 13 is made of Incone material. The sampling pipeline 13 made of Incone material is resistant to high temperature, material friction, and chlorine corrosion, which can ensure the service life of the sampling pipeline 13 in the environment of high temperature resistant materials, chlorine, and titanium tetrachloride, and can realize repeated sampling of the chlorination furnace, ensuring the normal use of the sampling device.

[0050] As an embodiment of the present invention, the sampling valve group includes at least a first high-temperature ball valve 2 and a second high-temperature ball valve 3, the negative extraction valve group includes at least a first carbon steel ball valve 5, the nitrogen valve group includes at least a second carbon steel ball valve 8, and the sample outlet valve group includes at least a third high-temperature ball valve 7. It should be understood that the sampling valve group is used to control the on-off of the sampling pipeline 13, and the sample outlet valve group is used to control the on-off of the sample outlet pipeline 14. Both need to be in direct contact with the high-temperature material taken out of the boiling chlorination furnace 1. The use of high-temperature ball valves can ensure the effectiveness of their use. The negative extraction valve group is used to control the on-off of the negative extraction pipeline 6, and the nitrogen valve group is used to control the on-off of the nitrogen pipeline 15. Both do not need to be in direct contact with the high-temperature material. The use requirements can be met by using carbon steel ball valves to avoid cost waste. At the same time, since the sampling valve group is in contact with the high-temperature material in the boiling chlorination furnace 1 for a long time, if only one high-temperature ball valve is set, it is easy to cause the high-temperature material and toxic gas in the boiling chlorination furnace 1 to leak out when it fails. Therefore, more than two high-temperature ball valves need to be set to ensure the safety of use and sampling of the boiling chlorination furnace 1.

[0051] As an embodiment of the present invention, a nitrogen flow meter 9 and a pressure gauge 10 are also provided on the nitrogen pipeline 15. The nitrogen flow meter 9 is used to control the flow rate of nitrogen, and the pressure gauge 10 is used to detect the pressure of nitrogen, so as to complete the purging of the sampler 4, the purging of the sampling pipeline 13, and the agitation of the material in the sampling port 12.

[0052] As a preferred embodiment, the nitrogen flow meter 9 is equipped with a magnetic filter, a check valve, and a needle valve (not shown in the figure). The magnetic filter is used to ensure the purity of the nitrogen to avoid contamination of the sample, and the check valve and the needle valve are used to prevent the cross-flow of high-temperature gas and materials into the nitrogen pipeline 15, and are also used to assist in regulating the nitrogen flow.

[0053] As an optional embodiment, the sampler 4 and / or the sampling barrel 11 are made of carbon steel. During the sampling process, the high-temperature material taken out has a certain temperature drop through the sampling pipeline 13, which will not damage the carbon steel material. At the same time, due to the existence of the negative extraction pipeline 6, the chlorine gas, titanium tetrachloride and other gases flowing out with the sampling are drawn away by the negative extraction pipeline 6, and will not cause corrosion to the sampler 4 and / or the sampling barrel 11. It should be noted that the harmful gases such as chlorine gas and titanium tetrachloride drawn out through the negative extraction pipeline 6 in this embodiment can be harmlessly treated by other methods of the prior art, which will not be limited or elaborated here.

[0054] Example 2

[0055] This embodiment provides an online sampling method for a high-temperature furnace bed of a large fluidized boiling chlorination furnace, which is used for the online sampling device as described in Example 1.

[0056] The sampling method comprises the following steps:

[0057] Step S1: Check that the sampling valve group, the negative extraction valve group, the nitrogen valve group, and the sample outlet valve group are all in a closed state;

[0058] Step S2: connecting the sample outlet pipeline 14 to discharge the material in the sampler 4;

[0059] Step S3: connecting the nitrogen pipeline 15, inputting nitrogen into the sampler 4 at a first preset pressure and a first preset flow rate, and purging the sampler 4;

[0060] Step S4: After the purging is completed, the sample outlet pipeline 14 and the nitrogen pipeline 15 are closed;

[0061] Step S5: sequentially connecting the nitrogen pipeline 15 and the sampling pipeline 13, delivering nitrogen at a first preset pressure and a first preset flow rate, so that the nitrogen purges the sampling pipeline 13 to keep it unobstructed;

[0062] Step S6: adjusting the nitrogen valve group to deliver nitrogen at a second preset pressure and a second preset flow rate to blow the material at the sampling port 12, and closing the nitrogen pipeline 15 after maintaining the nitrogen valve group for a first preset time;

[0063] Step S7: connecting the negative pressure extraction pipeline 6 to perform negative pressure extraction and depressurization on the sampler 4, and the high-temperature material in the boiling chlorination furnace 1 flows into the sampler 4 through the sampling pipeline 13 under the action of the pressure difference between the inside and outside of the furnace body;

[0064] Step S8: After the negative pressure is released for a second preset time, the negative pressure extraction pipeline 6 and the sampling pipeline 13 are closed;

[0065] Step S9: connecting the sample outlet pipeline 14 to guide the sample taken out from the sampler 4 into the sampling barrel 11;

[0066] Step S10: connecting the nitrogen pipeline 15, inputting nitrogen into the sampler 4 at a first preset pressure and a first preset flow rate, purging the sampler 4, and ensuring that the sample is completely released;

[0067] Step S11: sequentially connect the nitrogen pipeline 15 and the sampling pipeline 13, deliver nitrogen at a first preset pressure and a first preset flow rate, and allow the nitrogen to purge the sampling pipeline 13 to keep it unobstructed.

[0068] By the above steps, the online sampling of the boiling chlorination furnace 1 can be realized, to check the carbon ratio of the bed and the impurity content, timely adjust the mixed material feeding speed, or reduce the bed impurity content in the mode of deslagging, so as to effectively control the optimal fluidized reaction state in the furnace, ensure that the boiling chlorination reaction is carried out efficiently and steadily, and at the same time, the balanced material is added, the chlorine utilization efficiency is improved, and the cost loss caused by adding too much raw materials is reduced. In addition, the extraction of high-temperature materials is carried out by the described negative extraction pipeline 6, and airtight sampling is completed, and the risk of chlorine and titanium tetrachloride gas leakage is not all present in the process of sampling and setting out, which ensures the personal health of the operating personnel and is environmentally friendly. The determination method that the purging is completed and the sample is discharged completely in the step S4 is: there is no material discharge in the described sample outlet pipeline 14, and only gas is discharged.

[0069] As an optional embodiment of the present invention, when the boiling chlorination furnace 1 is not started, the steps S1-S4 are preparatory work before starting, and after the step S4 is completed, the boiling chlorination furnace 1 is started, and then the steps S5-S11 are performed to take samples. It should be understood that when the boiling chlorination furnace 1 is not started, the sampler 4 is cleaned first to avoid residual materials in the sampler 4 from contaminating the sampled sample.

[0070] As one embodiment, when multiple sampling is required, after the first sampling step S11 is completed, steps S5 to S11 are repeated. This setting can realize multiple sampling by the sampling device in a short period of time, and then the samples of multiple samplings are mixed together and sent for inspection, which can improve the accuracy of the test results and avoid the situation where the deviation of a single sampling is too large.

[0071] As an embodiment of the present invention, the first preset pressure is above 0.4 MPa, and the first preset flow rate is 5-10 m 3 / h, the second preset pressure is 0.4-0.6MPa, and the second preset flow rate is 15-20m 3 / h, the first preset time is 8-12 seconds, and the second preset time is 3-5 seconds. By setting the above preset values, the purging of the sampler 4, the purging of the sampling pipeline 13, the agitation of the high-temperature material of the sampling port 12 and the sampling of the high-temperature material are realized, and the online sampling work of the boiling chlorination furnace 1 is completed. The carbon ratio and impurity content of the bed can be checked, the feeding speed of the mixed material can be adjusted in time, or the impurity content of the bed can be reduced by means of slagging, etc., so as to effectively control the optimal fluidized reaction state in the furnace, ensure that the boiling chlorination reaction is carried out efficiently and smoothly, and at the same time, the material addition is balanced, the utilization efficiency of chlorine is improved, and the cost loss caused by excessive addition of raw materials is reduced.

[0072] Example 3

[0073] This embodiment provides an online sampling method for a high-temperature furnace bed of a large fluidized boiling chlorination furnace, which is used in the online sampling device described in Example 1 or the online sampling method described in Example 2.

[0074] Wherein, a movable sampling barrel 11 is provided at the outlet end of the sample outlet pipeline 14, and the sampling barrel 11 is used to hold the sample taken out by the sampling device, the sampling valve group at least includes a first high-temperature ball valve 2 and a second high-temperature ball valve 3, the negative suction valve group at least includes a first carbon steel ball valve 5, the nitrogen valve group at least includes a second carbon steel ball valve 8, the sample outlet valve group at least includes a third high-temperature ball valve 7, and a nitrogen flowmeter 9 and a pressure gauge 10 are also provided on the nitrogen pipeline 15. The sampling method comprises the following steps:

[0075] Step S1: Check that the first high-temperature ball valve 2, the second high-temperature ball valve 3, the first carbon steel ball valve 5, the second carbon steel ball valve 8, and the third high-temperature ball valve 7 are all in a closed state;

[0076] Step S2: Open the third high-temperature ball valve 7 to connect the sample outlet pipeline 14 and release the material in the sampler 4;

[0077] Step S3: Open the second carbon steel ball valve 8 to connect the nitrogen pipeline 15, and 3 / h flow rate of nitrogen into the sampler 4 to purge the sampler 4;

[0078] Step S4: After the purging is completed, close the third high-temperature ball valve 7 and the second carbon steel ball valve 8;

[0079] Step S5: Open the second carbon steel ball valve 8, the second high temperature ball valve 3 and the first high temperature ball valve 2 in sequence, connect the nitrogen pipeline 15 and the sampling pipeline 13, and conduct the nitrogen gas at a pressure of 0.4 MPa and 8 m 3 / h to deliver nitrogen gas so that the nitrogen gas purges the sampling pipeline 13 to keep the sampling pipeline 13 unobstructed;

[0080] Step S6: Adjust the second carbon steel ball valve 8 to 0.5 MPa pressure and 18 m 3 / h flow rate of nitrogen to blow the material at the sampling port 12, and then close the second carbon steel ball valve 8 after holding for 10 seconds;

[0081] Step S7: Open the first carbon steel ball valve 5 to connect the negative pressure extraction pipeline 6, and perform negative pressure extraction and depressurization on the sampler 4. The high-temperature material in the boiling chlorination furnace 1 flows into the sampler 4 through the sampling pipeline 13 under the action of the pressure difference between the inside and outside of the furnace body;

[0082] Step S8: After 4 seconds of negative pressure relief, close the first carbon steel ball valve 5, the second high-temperature ball valve 3 and the first high-temperature ball valve 2 to avoid excessive high-temperature material flowing out and ensure personal safety;

[0083] Step S9: Open the third high-temperature ball valve 7 to connect the sample outlet pipeline 14, and guide the sample taken out from the sampler 4 into the sampling barrel 11;

[0084] Step S10: Open the second carbon steel ball valve 8 to connect the nitrogen pipeline 15, and 3 / h flow rate of nitrogen into the sampler 4 to purge the sampler 4 to ensure that the sample is completely released;

[0085] Step S11: Open the second carbon steel ball valve 8, the second high temperature ball valve 3 and the first high temperature ball valve 2 in sequence, connect the nitrogen pipeline 15 and the sampling pipeline 13, and 3 / h to deliver nitrogen gas so that the nitrogen gas purges the sampling pipeline 13 to keep the sampling pipeline 13 unobstructed;

[0086] When multiple sampling is required, after the first sampling step S11, the steps S5 to S11 are executed in a loop; and the samples taken multiple times are discharged into the sampling barrel 11, mixed evenly, and then sent for inspection.

[0087] It should be noted that all the terms used in the present invention to indicate directionality and position, such as "upper", "lower", "left", "right", "front", "back", "vertical", "horizontal", "inner", "outer", "top", "lower", "tail end", "head end", "center", etc., are only used to explain the relative positional relationship and connection status between the components in a certain state, and are only for the convenience of describing the present invention, rather than requiring the present invention to be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the descriptions of "first", "second", etc. in the present invention are only used for descriptive purposes, and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of the indicated technical features.

[0088] Although the present invention is disclosed as above, the present invention is not limited thereto. Any person skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the scope defined by the claims.

Claims

1. A large-scale fluidized fluidized chlorination furnace high temperature furnace bed online sampling device, used for online sampling of a fluidized fluidized chlorination furnace (1), characterized in that: include: A sampling port (12) is provided on the boiling chlorination furnace (1), and the sampling port (12) is provided corresponding to the boiling section of the boiling chlorination furnace (1). The sampling port (12) is connected to a sampling pipeline (13), and a sampler (4) is connected to the other end of the sampling pipeline (13). The sampler (4) is also connected to a negative pressure extraction pipeline (6), a nitrogen pipeline (15), and a sample outlet pipeline (14). The negative pressure extraction pipeline (6) is used to extract negative pressure, and the nitrogen pipeline (15) is used to extract negative pressure. 15) is used to transport nitrogen to the sampler (4), and the sample outlet pipeline (14) is used to guide the sample taken out from the sampler (4). The sampling pipeline (13), the negative extraction pipeline (6), the nitrogen pipeline (15) and the sample outlet pipeline (14) are respectively provided with a sampling valve group, a negative extraction valve group, a nitrogen valve group and a sample outlet valve group, which are respectively used to control the on-off of the sampling pipeline (13), the negative extraction pipeline (6), the nitrogen pipeline (15) and the sample outlet pipeline (14); The sampling method of the sampling device comprises the following steps: Step S1: Check that the sampling valve group, the negative extraction valve group, the nitrogen valve group, and the sample outlet valve group are all in a closed state; Step S2: connecting the sample outlet pipeline (14) to discharge the material in the sampler (4); Step S3: connecting the nitrogen pipeline (15) and inputting nitrogen into the sampler (4) at a first preset pressure and a first preset flow rate to purge the sampler (4); Step S4: After the purging is completed, close the sample outlet pipeline (14) and the nitrogen pipeline (15); Step S5: sequentially connecting the nitrogen pipeline (15) and the sampling pipeline (13), delivering nitrogen at a first preset pressure and a first preset flow rate, so that the nitrogen purges the sampling pipeline (13) to keep it unobstructed; Step S6: adjusting the nitrogen valve group to deliver nitrogen at a second preset pressure and a second preset flow rate to blow the material at the sampling port (12), and closing the nitrogen pipeline (15) after maintaining the nitrogen at a first preset time; Step S7: connecting the negative pressure extraction pipeline (6) to negatively extract and depressurize the sampler (4); the high-temperature material in the boiling chlorination furnace (1) flows into the sampler (4) through the sampling pipeline (13) under the action of the pressure difference between the inside and outside of the furnace body; Step S8: After the negative pressure is released for a second preset time, the negative pressure extraction pipeline (6) and the sampling pipeline (13) are closed; Step S9: connecting the sample outlet pipeline (14) to guide the sample taken out from the sampler (4) into the sampling barrel (11); Step S10: connecting the nitrogen pipeline (15), inputting nitrogen into the sampler (4) at a first preset pressure and a first preset flow rate, and purging the sampler (4) to ensure that the sample is completely released; Step S11: sequentially connect the nitrogen pipeline (15) and the sampling pipeline (13), deliver nitrogen at a first preset pressure and a first preset flow rate, so that the nitrogen purges the sampling pipeline (13) to keep it unobstructed.

2. The large-scale fluidized boiling chlorination furnace high temperature hearth online sampling device as claimed in claim 1, characterized in that: A movable sampling barrel (11) is provided at the outlet end of the sample outlet pipeline (14), and the sampling barrel (11) is used to hold samples taken out by a sampling device.

3. The large-scale fluidized boiling chlorination furnace high temperature hearth online sampling device as claimed in claim 1 is characterized in that, The sampling pipeline (13) is made of Incone material.

4. The large-scale fluidized boiling chlorination furnace high temperature hearth online sampling device as claimed in claim 1, characterized in that: The sampling valve group comprises at least a first high-temperature ball valve (2) and a second high-temperature ball valve (3), the negative-pressure extraction valve group comprises at least a first carbon steel ball valve (5), the nitrogen valve group comprises at least a second carbon steel ball valve (8), and the sample outlet valve group comprises at least a third high-temperature ball valve (7).

5. The large-scale fluidized boiling chlorination furnace high temperature hearth online sampling device as claimed in claim 1 is characterized in that, A nitrogen flow meter (9) and a pressure gauge (10) are also provided on the nitrogen pipeline (15).

6. The large-scale fluidized boiling chlorination furnace high temperature hearth online sampling device as claimed in claim 5, characterized in that: The nitrogen flow meter (9) is equipped with a magnetic filter, a check valve and a needle valve.

7. A high-temperature furnace bed online sampling method, used for the online sampling device according to claim 1, characterized in that: When the boiling chlorination furnace (1) is not started, steps S1-S4 are preparatory work before starting. After step S4 is completed, the boiling chlorination furnace (1) is started, and then steps S5-S11 are performed to take samples.

8. The online sampling method according to claim 7, characterized in that: When multiple samplings are required, after the first sampling step S11 is completed, steps S5 to S11 are repeatedly executed.

9. The online sampling method according to claim 7, characterized in that: The first preset pressure is above 0.4 MPa, and the first preset flow rate is 5-10 m 3 / h, the second preset pressure is 0.4-0.6MPa, and the second preset flow rate is 15-20m 3 / h, the first preset time is 8-12 seconds, and the second preset time is 3-5 seconds.

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