阅读说明：本技术 一种基于x射线衍射分析的助熔剂添加控制系统及方法 (Flux adding control system and method based on X-ray diffraction analysis ) 是由 刘蓉 王晓龙 郜时旺 王琪 肖天存 于 2019-10-29 设计创作，主要内容包括：本发明公开的一种基于X射线衍射分析的助熔剂添加控制系统及方法,属于煤气化控制技术领域。包括煤灰取样器、煤灰进样器、X射线衍射仪、X射线衍射图谱分析仪、服务器和助熔剂进料器；煤灰取样器取样后通过煤灰进样器制样送入X射线衍射仪进行在线检测生成X射线衍射图谱,采用X射线衍射图谱分析仪对得到的X射线衍射图谱进行分析,服务器根据分析得到的数据实时生成助熔剂添加量调整策略,助熔剂进料器根据服务器所传输的助熔剂添加量调整策略确定助熔剂进料量进行添加,可实现助熔剂添加的在线实时控制,实现气化炉膜式水冷壁上正常的挂渣,保证气化炉长周期安全平稳运行,适用范围广,适于大规模推广。(The invention discloses a flux addition control system and method based on X-ray diffraction analysis, and belongs to the technical field of coal gasification control. The device comprises a coal ash sampler, a coal ash sample injector, an X-ray diffractometer, an X-ray diffraction pattern spectrum analyzer, a server and a fluxing agent feeder; the coal ash sampler samples and then sends the samples into an X-ray diffractometer through a coal ash sampler sample preparation device to perform online detection to generate an X-ray diffraction pattern, an X-ray diffraction pattern analyzer is adopted to analyze the obtained X-ray diffraction pattern, a server generates a flux addition amount adjusting strategy in real time according to data obtained by analysis, a flux feeder determines the flux feeding amount according to the flux addition amount adjusting strategy transmitted by the server to perform addition, online real-time control of flux addition can be realized, normal slag hanging on a film water-cooled wall of the gasification furnace is realized, long-period safe and stable operation of the gasification furnace is ensured, the application range is wide, and the method is suitable for large-scale popularization.)

1. A flux addition control system based on X-ray diffraction analysis is characterized by comprising a coal ash sampler (1), a coal ash injector (2), an X-ray diffractometer (3), an X-ray diffraction pattern spectrum analyzer (4), a server (5) and a flux feeder (6);

the coal ash sampler (1) is arranged at the outlet of the gasification furnace and is used for collecting coal ash and preparing the coal ash into a coal ash sample;

the coal ash sample injector (2) is used for sending the coal ash sample prepared by the coal ash sample injector (1) to the X-ray diffractometer (3);

the X-ray diffractometer (3) is connected with the X-ray diffraction pattern spectrum analyzer (4), and the X-ray diffractometer (3) is used for generating an X-ray diffraction pattern of the coal ash sample and sending the X-ray diffraction pattern to the X-ray diffraction pattern spectrum analyzer (4);

the coal ash sampler (1), the coal ash sample injector (2), the X-ray diffractometer (3), the X-ray diffractogram spectrum analyzer (4) and the fluxing agent feeder (6) are respectively connected with the server (5).

2. The flux addition control system based on X-ray diffraction analysis according to claim 1, wherein the coal ash sampler (1) comprises a sample loading device and a flattening device, wherein the sample loading device is used for containing collected coal ash, and the flattening device is used for flattening the coal ash in the sample loading device.

3. The flux addition control system based on X-ray diffraction analysis according to claim 1, characterized in that the scanning speed of the X-ray diffractometer (3) is 2 °/min, the scanning range is 10 ° to 60 °, and the scanning step is 0.02 °.

4. The system for controlling flux addition based on X-ray diffraction analysis according to claim 1, wherein the soot injector (2) is connected to a cooling system, and the cooling system is connected to the server (5).

5. The flux addition control system based on X-ray diffraction analysis according to claim 1, characterized in that the system further comprises a temperature measuring device for measuring the temperature of the soot sample, the temperature measuring device being connected to the server (5).

6. The flux addition control system according to claim 5, wherein the temperature measuring device is an infrared temperature measuring device.

7. The method for controlling the addition of the flux by using the flux addition control system based on the X-ray diffraction analysis as claimed in any one of claims 1 to 6, is characterized by comprising the following steps:

1) setting m₁The initial addition amount of the fluxing agent is used, and after the gasification reaction starts, the server (5) controls the coal ash sampler (1) to collect coal ash at the outlet of the gasification furnace and prepare a coal ash sample 1;

2) the server (5) controls the coal ash sample injector (2) to send the coal ash sample 1 to the X-ray diffractometer (3);

3) detecting the coal ash sample 1 by using an X-ray diffractometer (3) to obtain an X-ray diffraction pattern of the coal ash sample 1 and sending the X-ray diffraction pattern to an X-ray diffraction pattern spectrum analyzer (4);

4) an X-ray diffraction pattern analyzer (4) analyzes the X-ray diffraction pattern of the coal ash sample 1 to obtain the characteristic peaks of anorthite, forsterite and magnesia spinel in the X-ray diffraction pattern of the coal ash sample 1, and calculates the ratio a of the characteristic peak areas of anorthite, forsterite and magnesia spinel to the total peak area₁A is to₁Sending to a server (5);

5) the server (5) adjusts the amount of flux added in the flux feeder (6) to m₂，m₂＝2m₁The server (5) controls the coal ash sampler (1) to collect coal ash at the outlet of the gasification furnace and prepare a coal ash sample 2;

6) repeating the steps 2) to 4) to obtain the ratio a of the characteristic peak areas and the total peak area of anorthite, forsterite and magnesia spinel in the X-ray diffraction spectrum of the coal ash sample 2₂A is to₂Sending to a server (5);

7) server (5) pair a₁And a₂Making a comparison if a₂≤1.05a₁Maintaining the amount of the flux added m in the time period T₂(ii) a If a₂＞1.05a₁Repeating the steps 5) and 6) until a_n≤1.05a₁(n is 2,3,4 … …), the amount of flux added m is maintained during the time period T_n＝nm₁(n＝2,3,4……)；

8) Repeating the steps 1) to 7) at intervals of a time period T.

8. The carbon dioxide capture method of claim 7, wherein the flux is added in an initial amount m₁0.5-1% of coal feeding amount.

9. The method for capturing carbon dioxide according to claim 7, wherein the step 3) is performed by selecting 3 to 5 points on the surface of the coal ash sample and scanning each point 3 to 5 times.

10. The method for capturing carbon dioxide according to claim 7, wherein the time period T is 30 to 120 min.

Technical Field

The invention belongs to the technical field of coal gasification control, and particularly relates to a fluxing agent adding control system and method based on X-ray diffraction analysis.

Background

With the increasing shortage of domestic primary energy supply, the efficient utilization of the low-grade coal with high ash fusion temperature (ash melting point) more than 1500 ℃ is of great concern. The entrained flow bed gasification technology has strong adaptability to coal types, widens the utilization range of the coal types, and particularly can gasify the coal types with higher ash content. At present, the coal gasification technology develops towards high temperature and high pressure, the slag tapping gasification technology gradually takes the leading position to ensure that the gasification furnace can smoothly tap slag, and the operation temperature of the gasification furnace is higher than the flowing temperature of raw material coal in principle. Therefore, the carbon conversion rate cannot be reduced, normal slag adhering to the membrane water wall of the gasification furnace is smoothly realized, and the long-period safe and stable operation of the gasification furnace is ensured. The reserves of high ash point coal resources in China are large, wherein coal with an ash melting point of more than 1500 ℃ accounts for 50 percent of the total coal resources. In order to meet the requirement of the slagging-off gasification technology on ash melting point, a fluxing agent must be added to coal with high ash melting point temperature to effectively reduce the ash melting point.

The melting point of coal ash is an important index of coal for gasification, and guides the addition of a specific gasifier fluxing agent. The melting point of coal ash depends largely on the chemical composition of the coal ash and its content. Therefore, the amount of flux to be added needs to be determined by studying the chemical composition of the coal ash in detail. Alumina, silica are generally called as acid oxides, the content of which is higher, the melting point temperature of coal ash is higher, magnesia, calcium oxide and iron oxide are generally called as alkaline oxides, the content of which is higher, the melting point temperature of coal ash is lower, but in view of the complexity of chemical components of coal ash in the actual production process and certain fluctuation of the content of each chemical component, a rapid coal ash chemical component analysis method is needed for real-time online analysis, and the adding type and adding amount of the fluxing agent are determined according to the analysis method.

The existing method for analyzing elements such as Ca, Mg and the like in coal ash mainly adopts a titration analysis method, has complicated steps and long time consumption, and cannot realize on-line measurement. The kind and amount of flux added cannot be adjusted on-line according to actual conditions.

Disclosure of Invention

In order to solve the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a flux addition control system and method based on X-ray diffraction analysis, which can quickly and accurately detect the components of coal ash, thereby guiding the addition of the flux to the gasifier.

The invention is realized by the following technical scheme:

the invention discloses a fluxing agent adding control system based on X-ray diffraction analysis, which comprises a coal ash sampler, a coal ash sample injector, an X-ray diffractometer, an X-ray diffraction pattern spectrum analyzer, a server and a fluxing agent feeder, wherein the coal ash sampler is connected with the coal ash sample injector;

the coal ash sampler is arranged at the outlet of the gasification furnace and is used for collecting coal ash and preparing the coal ash into a coal ash sample;

the coal ash sample injector is used for sending a coal ash sample to the X-ray diffractometer;

the X-ray diffractometer is connected with the X-ray diffraction pattern spectrum analyzer and is used for generating an X-ray diffraction pattern of the coal ash sample and sending the X-ray diffraction pattern to the X-ray diffraction pattern spectrum analyzer;

the coal ash sampler, the coal ash injector, the X-ray diffraction pattern analyzer and the fluxing agent feeder are respectively connected with the server.

Preferably, the coal ash sampler comprises a sample loading device and a flattening device, wherein the sample loading device is used for containing the collected coal ash, and the flattening device is used for flattening the coal ash in the sample loading device.

Preferably, the scanning speed of the X-ray diffractometer is 2 DEG/min, the scanning range is 10 DEG-60 DEG, and the scanning step is 0.02 deg.

Preferably, the soot injector is connected to a cooling system.

Preferably, the system further comprises a temperature measuring device for measuring the temperature of the coal ash sample.

Further preferably, the temperature measuring device is an infrared temperature detector.

The invention also discloses a method for controlling the addition of the fluxing agent by adopting the fluxing agent addition control system based on the X-ray diffraction analysis, which comprises the following steps:

1) setting m₁The initial addition amount of the fluxing agent is used, and after the gasification reaction starts, the server controls the coal ash sampler to collect coal ash at the outlet of the gasification furnace and prepare a coal ash sample 1;

2) the server controls the coal ash sample injector to send the coal ash sample 1 to the X-ray diffractometer;

3) detecting the coal ash sample 1 by using an X-ray diffractometer to obtain an X-ray diffraction pattern of the coal ash sample 1 and sending the X-ray diffraction pattern to an X-ray diffraction pattern analyzer;

4) analyzing the X-ray diffraction pattern of the coal ash sample 1 by an X-ray diffraction pattern analyzer to obtain the characteristic peaks of anorthite, forsterite and magnesia spinel in the X-ray diffraction pattern of the coal ash sample 1, and calculating the ratio a of the characteristic peak areas to the total peak area of the anorthite, forsterite and magnesia spinel₁A is to₁Sending the data to a server;

5) the amount of flux added to the flux feeder was adjusted to m by the server₂，m₂＝2m₁The server controls the coal ash sampler to collect coal ash at the outlet of the gasification furnace and prepares a coal ash sample 2;

6) repeating the steps 2) to 4) to obtain the ratio a of the characteristic peak areas and the total peak area of anorthite, forsterite and magnesia spinel in the X-ray diffraction spectrum of the coal ash sample 2₂A is to₂Sending the data to a server;

7) server pair a₁And a₂Making a comparison if a₂≤1.05a₁Maintaining the amount of the flux added m in the time period T₂(ii) a If a₂＞1.05a₁Repeating the steps 5) and 6) until a_n≤1.05a₁(n is 2,3,4 … …), the amount of flux added m is maintained during the time period T_n＝nm₁(n＝2,3,4……)；

8) Repeating the steps 1) to 7) at intervals of a time period T.

Preferably, the initial amount m of the flux added is₁0.5-1% of coal feeding amount.

Preferably, in the detection in the step 3), 3-5 points are selected on the surface of the coal ash sample, and each point is scanned for 3-5 times.

Preferably, the time period T is 30-120 min.

Compared with the prior art, the invention has the following beneficial technical effects:

according to the flux addition control system based on X-ray diffraction analysis, a coal ash sampler samples and then sends the sampled sample into an X-ray diffractometer for on-line detection to generate an X-ray diffraction pattern, so that the accuracy is high, and the speed is high; the obtained X-ray diffraction pattern is analyzed by adopting an X-ray diffraction pattern analyzer, a server generates a flux addition amount adjusting strategy in real time according to data obtained by analysis, a flux feeder determines flux feeding amount according to the flux addition amount adjusting strategy transmitted by the server for adding, online real-time control of flux addition can be realized, normal slag hanging on a gasifier membrane water wall is realized, and long-period safe and stable operation of the gasifier is ensured. The method is applicable to various coals with the coal ash melting point within 1000-1500 ℃, is applicable to various entrained flow gasification technologies such as Shell, GSP, HT-L and GE, has wide application range and is suitable for large-scale popularization.

Furthermore, the coal ash discharged from the gasification furnace is collected through the sample loading device and the flattening device, and a coal ash sample with a flat surface is prepared, so that the data obtained by scanning of the X-ray diffractometer is more accurate.

Furthermore, the coal ash sample injector is connected with a cooling system, so that the coal ash sample can be rapidly cooled to the working temperature of the X-ray diffractometer, and the online detection efficiency of the system is improved.

Further, the system is provided with the temperature measuring device who is used for measuring coal ash sample temperature, can detect the real-time temperature of coal ash sample and send to the server, starts X-ray diffractometer when reaching X-ray diffractometer's operating temperature, and degree of automation is high, and the data that record are accurate.

Furthermore, the temperature measuring device adopts an infrared temperature measurer, can remotely measure the temperature of the surface of the coal ash sample, and has the advantages of quick response time, non-contact, safe use, long service life and the like.

The invention discloses a method for controlling the addition of a fluxing agent by adopting the fluxing agent addition control system based on X-ray diffraction analysis, which comprises the steps of firstly determining the initial addition amount of the fluxing agent according to an empirical value, and measuring the ratio of the characteristic peak areas and the total peak area of anorthite, forsterite and magnesium spinel; and then increasing the addition amount of the cosolvent by one time, measuring the ratio of the characteristic peak areas of anorthite, forsterite and magnesium spinel to the total peak area again, comparing the results obtained by two measurements, and when the fluctuation of the obtained numerical value is less than 5%, considering that the melting point of the coal ash can not be obviously increased by continuously adding the cosolvent, integrating economic factors and maintaining the addition amount of the cosolvent at the moment. The method is simple and convenient to operate, combines experience and an actually made flux addition amount adjusting strategy, is simple and convenient, high in speed and accuracy, high in automation degree, and capable of playing a role in guiding the addition of the flux of the specific gasification furnace.

Further, the initial amount m of the flux added₁The amount of the coal is 0.5% -1% of the coal feeding amount, and the coal feeding amount is a value determined according to an empirical value, so that the system can rapidly determine the final addition amount of the fluxing agent.

Furthermore, during detection, multiple points on the surface of the coal ash sample are detected for multiple times, which is beneficial to improving the accuracy of the test.

Furthermore, 30-120 min is selected as a time period for repeated measurement, which is beneficial to adjusting the addition amount of the fluxing agent at any time along with fluctuation of coal types.

Drawings

FIG. 1 is a schematic diagram of the overall structure of a flux addition control system based on X-ray diffraction analysis according to the present invention;

fig. 2 is a schematic workflow diagram of the flux addition control system based on X-ray diffraction analysis according to the present invention.

In the figure: 1-coal ash sampler, 2-coal ash injector, 3-X-ray diffractometer, 4-X-ray diffractometer analyzer, 5-server and 6-fluxing agent feeder.

Detailed Description

The invention will now be described in further detail with reference to the following drawings and specific examples, which are intended to be illustrative and not limiting:

FIG. 1 is a control system for flux addition based on X-ray diffraction analysis, which comprises a coal ash sampler 1, a coal ash injector 2, an X-ray diffractometer 3, an X-ray diffractogram analyzer 4, a server 5 and a flux feeder 6;

the coal ash sampler 1 is arranged at the outlet of the gasification furnace, the coal ash sampler 1 comprises a sample loading device and a flattening device, the sample loading device is used for containing collected coal ash, the sample loading device can be a round container with a certain depth, and the flattening device is used for flattening the coal ash in the sample loading device to prepare a round cake-shaped coal ash sample.

The coal ash sample injector 2 is used for delivering the coal ash sample prepared by the coal ash sample injector 1 to the X-ray diffractometer 3, and the coal ash sample injector 2 can adopt a conveying device commonly used in an automatic system, such as a conveying belt, a conveying table, a mechanical arm and the like; the coal ash injector 2 is connected with a cooling system, and the cooling system is connected with the server 5. The system also comprises a temperature measuring device for measuring the temperature of the coal ash sample, the temperature measuring device is connected with the server 5, and an infrared temperature measurer is preferably selected as the temperature measuring device.

The X-ray diffractometer 3 is connected with the X-ray diffraction pattern spectrum analyzer 4, the X-ray diffractometer 3 is used for generating an X-ray diffraction pattern of the coal ash sample and sending the X-ray diffraction pattern to the X-ray diffraction pattern spectrum analyzer 4, and the parameters of the X-ray diffractometer 3 are preferably as follows: the scanning speed is 2 degrees/min, the scanning range is 10 degrees to 60 degrees, and the scanning step is 0.02 degrees;

the coal ash sampler 1, the coal ash injector 2, the X-ray diffractometer 3, the X-ray diffraction pattern analyzer 4 and the flux feeder 6 are respectively connected to a server 5.

As shown in fig. 2, the method for controlling the flux addition by using the flux addition control system based on the X-ray diffraction analysis comprises the following steps:

1) setting m₁The initial amount of the flux is generally m₁0.5% -1% of coal feeding quantity, gasifyingAfter the reaction starts, the server 5 controls the coal ash sampler 1 to collect coal ash at the outlet of the gasification furnace and prepare a coal ash sample 1;

2) the server 5 controls the coal ash sample injector 2 to send the coal ash sample 1 to the X-ray diffractometer 3;

3) detecting the coal ash sample 1 by using an X-ray diffractometer 3, selecting 3-5 points on the surface of the coal ash sample, scanning each point for 3-5 times to obtain an X-ray diffraction pattern of the coal ash sample 1, and sending the X-ray diffraction pattern to an X-ray diffraction pattern spectrum analyzer 4;

4) an X-ray diffraction pattern analyzer 4 analyzes the X-ray diffraction pattern of the coal ash sample 1 to obtain the characteristic peaks of anorthite, forsterite and magnesia spinel in the X-ray diffraction pattern of the coal ash sample 1, and calculates the ratio a of the characteristic peak areas to the total peak area of the anorthite, forsterite and magnesia spinel₁A is to₁Sending to the server 5;

5) the server 5 adjusts the amount of flux added to the flux feeder 6 to m₂，m₂＝2m₁The server 5 controls the coal ash sampler 1 to collect coal ash at the outlet of the gasification furnace and prepare a coal ash sample 2;

6) repeating the steps 2) to 4) to obtain the ratio a of the characteristic peak areas and the total peak area of anorthite, forsterite and magnesia spinel in the X-ray diffraction spectrum of the coal ash sample 2₂A is to₂Sending to the server 5;

7) server 5 to a₁And a₂Making a comparison if a₂≤1.05a₁Maintaining the amount of the flux added m in the time period T₂(ii) a If a₂＞1.05a₁Repeating the steps 5) and 6) until a_n≤1.05a₁(n is 2,3,4 … …), the amount of flux added m is maintained during the time period T_n＝nm₁(n＝2,3,4……)；

8) And repeating the steps 1) to 7) at intervals of a time period T, wherein T is usually 30-120 min.

A above₁，a₂……a_n(n-2, 3 … …) is calculated by the X-ray diffraction pattern analyzer 4 by a₁＝a_n＝I_{Calcium lengthStone (stone)}+I_{Olivine stone}+I_Spinel(n-2, 3 … …) wherein the peak area ratio I_Anorthite＝S_{Calcium feldspar-}S_{General assembly}，I_{Olivine stone}＝S_{Olive stone/liver and/or kidney combination}S_{General assembly}，I_Spinel＝S_Spinel-S_{General assembly}In which S is_AnorthiteThe characteristic peak area of anorthite at 2 theta of 26.9-27.9 DEG, S_{Olivine stone}The characteristic peak area of the olivine at 2 theta of 36.3-35.3 DEG, S_SpinelThe characteristic peak area of the spinel at 2 theta of 36.6-36.95 DEG is calculated to obtain the peak area ratio I_Anorthite＝S_{Calcium feldspar-}S_{General assembly}，I_{Olivine stone}＝S_{Olive stone/liver and/or kidney combination}S_{General assembly}，I_Spinel＝S_Spinel-S_{General assembly}. Wherein S is_{General assembly}＝S_Anorthite+S_{Olivine stone}+S_Spinel。

The invention is further explained below in the context of several specific application examples: