CN111077037B - Online integrated continuous and rapid determination device and method for moisture and ash content - Google Patents
Online integrated continuous and rapid determination device and method for moisture and ash content Download PDFInfo
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- CN111077037B CN111077037B CN201911404137.2A CN201911404137A CN111077037B CN 111077037 B CN111077037 B CN 111077037B CN 201911404137 A CN201911404137 A CN 201911404137A CN 111077037 B CN111077037 B CN 111077037B
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Abstract
The invention discloses a device and a method for online integrated continuous and rapid determination of moisture and ash. The measuring method comprises the steps of placing a crude sample in a large corundum hanging basket, placing corresponding distribution plate grooves, heating the hanging basket at a temperature range of about 150 ℃, introducing nitrogen to the hanging basket until the quality is constant, then sending the sample into a temperature range of about 820 ℃, switching to introduce air until the quality is constant, automatically obtaining a weight loss curve, obtaining the moisture content and the ash content, and completing the whole process within half an hour according to different samples. The method has the advantages of capability of measuring the moisture and ash content of a large sample (more than or equal to 100 mg) in real time in a large-scale process, high measuring speed (the powdered coal sample can be finished within ten minutes), convenient operation and low equipment cost.
Description
Technical Field
The invention relates to a device and a method for online integrated continuous and rapid determination of moisture and ash, in particular to a device and a method for continuously and rapidly determining solid samples such as coal, coke, fine powder, ash and the like which have high moisture content, poor carbon residue reactivity and are difficult to burn through in industry.
Background
In the related industries and process test processes of various coals and biomasses, the moisture and ash content of substances need to be monitored in real time so as to quickly calculate the carbon balance, and further, corresponding process conditions are adjusted so as to improve the yield and the working efficiency. The larger the weight of the sampled sample is, the stronger the representativeness is, but the longer the corresponding measuring time is, the invention is designed to rapidly analyze the moisture and the ash content of the industrial sample in real time aiming at the problem. The measurement of the moisture and the ash content is based on the national standard GB/T212, and the measurement principle is as follows: and weighing the variable quantity of the test sample mass at a constant temperature for a certain time until the sample mass does not change any more. The method is a detection standard of all measuring instruments, but has the defects of complex operation, incapability of continuously measuring moisture and ash content, long time consumption and the like, can not realize rapid and continuous sample measurement, and can not meet the requirement of rapid measurement of some parameters in the process of a process test. The industrial analyzer used in the laboratory can continuously and variously measure the moisture, the ash content and the volatile matter, but the measuring time is longer, 1-2 hours are needed, the measuring time for the sample which has large water content and is difficult to burn through in the actual industry is longer, and the accuracy is poor; and only <100mg of sample analysis, not representative. And foreign instruments with high measurement quantity are expensive in price and long in measurement time, and are not suitable for industrial requirements.
Disclosure of Invention
The invention aims to provide an online integrated moisture and ash continuous and rapid determination device and method with low determination cost, rapidness and accuracy and continuous sample determination aiming at the characteristics of high content of discharged slag moisture, poor reactivity of carbon residue and difficult thorough burning in the large-scale coal gasification and coal pyrolysis process test process and the defects of the moisture and ash determination technology for monitoring solid samples in real time in the existing industrial test.
According to the invention, the large sample amount is measured according to the measurement principle of the national standard GB/T212, and a set of rapid, accurate and low-cost moisture and ash content measurement device is designed, so that the requirement of real-time monitoring in industry is met.
The invention provides an online integrated continuous and rapid moisture and ash content measuring device which comprises a balance, a suspension wire, a reaction tube, a hanging basket, a distribution plate groove, an electric furnace, a thermocouple sleeve (a thermocouple is arranged in the sleeve), a support frame, an air inlet pipe and a lifter, wherein the balance, the suspension wire, the reaction tube, the hanging basket, the distribution plate groove, the electric furnace, the thermocouple, the support frame, the air inlet pipe and the lifter are sequentially arranged from top to bottom in the whole device, and the reaction tube, the electric furnace and the lifter are connected; the electronic balance and the lifter are controlled by a computer, the position of the lifter is controlled, the scale reading is automatically recorded, a moisture and ash temperature measuring interval is determined according to a thermocouple, the position is recorded by a numerical control component, and temperature calibration is carried out; and obtaining a weight loss curve and the contents of water and ash.
In the device, a thermocouple is arranged in the reaction tube, and the temperature control program is used for carrying out temperature programmed heating through a temperature controller; the distribution plate is arranged in the reaction tube so as to control the influence of the airflow on the weighing object.
In the device, the balance is arranged above the balance support frame, and the base of the balance support frame is connected with the heat insulation plate.
In the device, the electric furnace supporting plate is arranged at the bottom of the electric furnace, the elevator supporting plate is arranged at the bottom of the elevator, and the elevator base is arranged below the elevator supporting plate.
In the device, the analytical balance and the lifter are provided with signal interfaces which are connected with a computer to collect weight change signals, so that the computer can automatically control weight signals and position signals; when the sample is measured, the temperature interval in the reaction furnace is calibrated by a standard thermocouple, and the position of the corundum hanging basket is determined by the computer through automatic control and recording of the lifter.
In the device, a thermocouple is arranged in the reaction tube, the temperature control program is programmed to be heated by a temperature control instrument, and a distribution plate groove is arranged in the reaction tube so as to control the influence of the airflow on a weighing object.
In the device, the distribution plate groove arranged in the reaction tube is made of 2520 steel sheets, a hole with the diameter of 0.5cm is formed in the center of the bottom of the groove, the distribution plate groove is formed by splicing two semicircular grooves for convenient placement, a semicircular hole is formed in the center of the bottom of each semicircular groove, and a circular hole is formed in the bottom of the distribution plate groove formed by splicing the two semicircular grooves.
In the device, a plurality of small holes are distributed on the edge of the groove base of the symmetrically cut distribution plate in the reaction tube, and the diameter and the number of the holes are determined according to an actual measurement sample to determine the zero point of the electronic balance to keep stable. Further, the diameter of the hole is 0.1 cm-1.0 cm.
In the device, the suspension wire is connected to the lower part of the balance and is a platinum wire or a high-temperature thermocouple wire, the weighing basket is a corundum basket, and the specific model is determined by a measured sample.
The invention provides a method for rapidly measuring the moisture content and the ash content of a sample in a test process by adopting the device, which comprises the following operation steps: sequentially and continuously measuring the moisture and the ash content in the same measuring device, placing a certain amount of coal sample in a corundum hanging basket in the device, automatically reading the initial mass of the sample, placing the corresponding distribution plate groove, heating to a temperature range of 150 ℃, and introducing nitrogen with constant drying flow rate until the mass is constant; then, the sample is sent into a temperature region of 820 ℃, air with constant drying flow rate is introduced, the sample is heated and burned until the quality is constant, then the whole weight loss curve is obtained, and the moisture content and the ash content are calculated.
The invention provides a device and a method for rapidly measuring moisture and ash content in coal and coke, which are applied to large-scale industrial process tests, and specifically comprises the following steps:
(1) firstly, calibrating a temperature interval by using a standard thermocouple, measuring the moisture at about 150 ℃, measuring the ash at about 820 ℃, determining the position of the elevator, and automatically recording by using a computer;
(2) placing a distribution plate groove in a reaction tube, adjusting the flow rate of gas (nitrogen or air), selecting a proper distribution plate groove, and determining the zero point of an analytical balance;
(3) placing a certain amount of coarse coal sample in a corundum hanging basket in the device, automatically reading the initial mass of the sample, placing the sample in the groove of the distribution plate selected in the step (2), heating to a temperature range of 150 ℃, and introducing nitrogen with constant drying flow rate (20 ml/min) into the reaction furnace through an air inlet pipe until the mass is constant as displayed by a computer;
(4) after the quality is constant in the step (2), the hanging basket is lifted to the temperature range of 820 ℃, gas is changed into air with constant drying flow rate (20 ml/min), and reaction is carried out until the quality is constant as displayed by a computer;
(5) thus obtaining the weight loss curve of the whole sample, automatically calculating the contents of water and ash, and measuring the time for less than 30 min.
The invention has the beneficial effects that:
the invention designs and develops a rapid industrial analysis device aiming at the characteristics of high content of discharged slag and water, poor reactivity of carbon residue and difficult thorough burning in the test process of large-scale coal gasification and coal pyrolysis process, and solves the problem of rapid industrial analysis of solid samples in the pilot-scale test and industrial demonstration process.
Secondly, a large amount of solid coarse samples are used for measurement, and the device has more representativeness than the existing measurement device, and the reliability of data is improved. Most of the existing finished product measuring instruments can only analyze milligram-level samples, but are not representative, and instruments with high measuring quantity are expensive and long in measuring time, so that the existing finished product measuring instruments are not suitable for industrial requirements.
The parts and accessories of the whole measuring device are simple and easy to obtain, the price is low, and the requirements of industrial factories are met.
The method has the advantages of being capable of measuring the moisture and ash content of the sample in real time in a large-scale process, quickly calculating the carbon balance, further adjusting corresponding process conditions, improving the yield and the working efficiency, being high in measuring speed (the powdery coal sample can be finished within ten minutes), being convenient to operate and low in equipment cost.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
Fig. 2 is a three-dimensional view of the groove (half) structure of the distribution plate of the device of the present invention.
Fig. 3 is a perspective view of the groove (half) of the distribution plate of the device of the present invention.
In the figure, the device comprises a balance 1, a balance 2, a balance support frame 3, a heat insulation plate 4, a suspension wire 5, a corundum hanging basket 6, a distribution plate groove 7, a reaction tube 8, a support frame 9, an electric furnace 10, a thermocouple sleeve 11, an electric furnace support plate 12, an air inlet pipe 13, an electric furnace support column 14, a lifter support plate 15 and a lifter.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
As shown in FIGS. 1-2, an on-line integrated continuous rapid measuring device for moisture and ash content mainly comprises a lifting component, a heating component, a temperature control component, a sample weighing component, a supporting component and a numerical control component. The device specifically comprises a balance 1, a balance support frame 2, a heat insulation plate 3, a suspension wire 4, a corundum hanging basket 5, a distribution plate groove 6, a reaction tube 7, a support frame 8, an electric furnace 9, a thermocouple sleeve 10, an electric furnace support plate 11, an air inlet pipe 12, an electric furnace support column 13, a lifter support plate 14 and a lifter 15. Wherein, a standard thermocouple is used for determining the temperature measuring interval of the moisture and the ash, and a numerical control part is used for recording the position and carrying out temperature calibration. Wherein the reaction tube 7, the electric furnace 9 and the lifter 15 are connected; the lower surface of the electronic balance 1 is connected with a suspension wire 4 and a corundum hanging basket 5, the electronic balance 1 and the lifter 15 are controlled by a computer, the position of the lifter is controlled, the scale reading is automatically recorded, and a weight loss curve and the moisture and ash content are obtained.
The analytical balance 1 and the lifter 15 are provided with signal interfaces and are connected with a computer to collect weight change signals, so that the weight signals and position signals can be automatically controlled by the computer. When the sample is measured, the temperature interval in the reaction furnace is calibrated by a standard thermocouple, and the position of the corundum hanging basket 5 is determined by the computer automatically controlled and recorded by the lifter 15.
A thermocouple is arranged in a reaction tube of the device, temperature control program is used for carrying out temperature program heating through a temperature control instrument, and a distribution plate groove 6 is arranged in a reaction tube 7 so as to control the influence of airflow on a weighing object.
The groove of the distribution plate arranged in the reaction tube is made of 2520 steel sheets, dots at the bottom of the groove are provided with holes with the diameter of 0.5cm, and then the holes are symmetrically cut along the diameter of the bottom and are divided into two parts.
A plurality of small holes are distributed on the edge of the base of the symmetrically cut distribution plate groove 6 in the reaction tube 7, the hole diameter and the hole number (the hole diameter is 0.1 cm-1.0 cm) are determined according to an actual measurement sample, and the zero point of the electronic balance is determined to be kept stable.
The on-line integrated continuous and rapid measuring device for the moisture and the ash content is characterized in that a platinum wire or a high-temperature thermocouple wire is connected below a balance, a weighing hanging basket is a corundum hanging basket, and the specific model is determined by a measuring sample.
The method for rapidly measuring the moisture content and the ash content of the sample in the process of the process test is characterized in that the moisture content and the ash content are sequentially and continuously measured in the same measuring device, a certain amount of coal sample is placed in a corundum hanging basket in the device, after the initial mass of the sample is automatically read, a corresponding distribution plate groove is placed, the temperature is raised to a temperature interval of 150 ℃, and nitrogen with constant drying flow rate is introduced until the mass is constant; then, the sample is sent into a temperature region of 820 ℃, air with constant drying flow rate is introduced, the sample is heated and burned until the quality is constant, then the whole weight loss curve is obtained, and the moisture content and the ash content are calculated.
And respectively measuring the moisture and the ash content of the experimental Shenmu bituminous coal, the slag sample with large water content and the fine powder in the coal gasification test process.
Example 1:
the method for measuring moisture and ash content of experimental nakedful coal comprises the following steps:
(1) before the test is started, a temperature interval is firstly calibrated by using a standard thermocouple, the moisture content is measured at about 150 ℃, the ash content is measured at about 820 ℃, and the position of the elevator is determined and recorded by a computer;
(2) placing a distribution plate groove in a reaction tube, adjusting the flow rate (20 ml/min) of gas (nitrogen or air), selecting the distribution plate groove with the aperture of 0.7cm when the mesh number of raw coal is below 2.5mm, determining the zero point of an analytical balance, and taking out the groove.
(3) Placing a crude coal sample of about 700mg in a corundum hanging basket in the device, automatically reading the initial mass of the sample, placing the sample in the groove of the distribution plate selected in the step (2), heating to a temperature range of 150 ℃, and introducing nitrogen with constant drying flow rate (20 ml/min) into the reaction furnace through an air inlet pipe until the mass is constant as displayed by a computer;
(4) after the quality is constant in the step (2), the hanging basket is lifted to the temperature range of 820 ℃, gas is changed into air with constant drying flow rate (20 ml/min), and reaction is carried out until the quality is constant as displayed by a computer;
(5) thus obtaining the weight loss curve of the whole sample, automatically calculating the contents of water and ash, and measuring the time for less than 20 min.
The measured results are compared with the national standard measurement GB/T212 as follows:
TABLE 1
Example 2:
and (3) measuring the moisture and ash content of the generated slag sample with large water content, selecting the slag sample with large water content in the step (2), selecting a distribution plate groove with the depth of 0.5cm, and determining the zero point of the balance, wherein the rest steps are the same as the first embodiment. The determination time is less than 30min, and the determination result is compared with the national standard determination as follows:
TABLE 2
Example 3:
for most of the fine powder samples smaller than 0.5mm, 1cm of the groove of the distribution plate was selected in step (2), the zero point of the analytical balance was determined, and the rest of the procedure was the same as in example one. The determination time is less than 10min, and the determination result is compared with the national standard determination as follows:
TABLE 3
The comparison of the three embodiments shows that the speed of measuring a large amount of solid samples by the device is higher than that of a national standard method, and data can be provided in the continuous industrial test operation; for samples with coarser particles, the larger the error, the longer it takes.
The above detailed description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the present invention. All equivalent changes and modifications made according to the claims of the present invention should fall within the scope of the present invention.
Claims (9)
1. The utility model provides a continuous spot test device of online integration of moisture ash content which characterized in that: the device comprises an analytical balance, a suspension wire, a reaction tube, a hanging basket, a distribution plate groove, an electric furnace, a thermocouple sleeve, a balance support frame, an air inlet tube and a lifter, wherein the analytical balance, the balance support frame, the suspension wire, the hanging basket, the distribution plate groove, the reaction tube, the electric furnace, a thermocouple, the air inlet tube and the lifter are sequentially arranged from top to bottom; the lower part of the analytical balance is connected with a suspension wire and a hanging basket, the analytical balance and a lifter are controlled by a computer, the position of the lifter is controlled, the reading of the analytical balance is automatically recorded, a moisture and ash temperature measuring interval is determined according to a thermocouple, the position is recorded by a numerical control part, and temperature calibration is carried out; obtaining a weight loss curve and the contents of water and ash;
the reaction tube is internally provided with a distribution plate groove so as to control the influence of the airflow on the weighing object; a hole with the diameter of 0.5cm is formed in the center of the bottom of the groove;
the hanging basket is located outside the electric furnace and above the reaction tube, and the elevator drives the reaction tube and the electric furnace to lift.
2. The on-line integrated continuous rapid moisture and ash content measuring device according to claim 1, characterized in that: a thermocouple is arranged in the reaction tube and is arranged in a thermocouple sleeve, and the temperature control program is programmed through a temperature control instrument.
3. The on-line integrated continuous rapid moisture and ash content measuring device according to claim 2, characterized in that: the distribution plate groove arranged in the reaction tube is made of 2520 steel sheets and is formed by splicing two semicircular grooves.
4. The on-line integrated continuous rapid moisture and ash content measuring device according to claim 3, characterized in that: and a plurality of small holes are distributed at the edge of the base of the groove of the distribution plate, and the diameter of each hole is 0.1 cm-1.0 cm.
5. The on-line integrated continuous rapid moisture and ash content measuring device according to claim 1, characterized in that: the analytical balance and the lifter are provided with signal interfaces and are connected with a computer to collect weight change signals, so that the weight signals and position signals can be automatically controlled by the computer; when the sample is measured, the temperature interval in the electric furnace is calibrated by a standard thermocouple, and the position of the hanging basket is determined by the elevator under the automatic control and record of the computer.
6. The on-line integrated continuous rapid moisture and ash content measuring device according to claim 1, characterized in that: the hanging wire is connected below the analytical balance and is a platinum wire or a high-temperature thermocouple wire, the hanging basket is a corundum hanging basket, and the specific model is determined by a measured sample.
7. The on-line integrated continuous rapid moisture and ash content measuring device according to claim 1, characterized in that: the analytical balance is arranged above the balance support frame, and the base of the balance support frame is connected with the heat insulation plate; an electric furnace supporting plate is arranged at the bottom of the electric furnace; the bottom of the elevator is provided with an elevator supporting plate, and an elevator base is arranged below the elevator supporting plate.
8. An online integrated continuous rapid determination method for moisture and ash, which adopts the online integrated continuous rapid determination device for moisture and ash as claimed in any one of claims 1 to 7, and is characterized in that: sequentially and continuously measuring the moisture and the ash content in the same measuring device, placing a coal sample in a hanging basket, automatically reading the initial mass of the sample, placing a corresponding distribution plate groove, heating to a temperature range of 150 ℃, and introducing nitrogen with constant drying flow rate until the mass is constant; then, the sample is sent into a temperature region of 820 ℃, air with constant drying flow rate is introduced, the sample is heated and burned until the quality is constant, then the whole weight loss curve is obtained, and the moisture content and the ash content are calculated.
9. The on-line integrated continuous and rapid determination method of moisture and ash content according to claim 8, characterized by comprising the following steps:
(1) firstly, calibrating a temperature interval by using a standard thermocouple, measuring the moisture at 150-200 ℃ and the ash at 810-830 ℃, determining the position of the elevator, and automatically recording by using a computer;
(2) placing a distribution plate groove in the reaction tube, adjusting the flow rate of nitrogen or air, selecting a proper distribution plate groove, and determining the zero point of the analytical balance;
(3) placing a coarse coal sample in a corundum hanging basket in the device, automatically reading the initial mass of the sample, then placing the sample into the groove of the distribution plate selected in the step (2), heating the sample to a temperature range of 150 ℃, and introducing nitrogen with the drying flow rate of 20ml/min into the reaction furnace through an air inlet pipe until the mass is constant as displayed by a computer;
(4) after the quality is constant in the step (3), the hanging basket is lifted to the temperature range of 820 ℃, gas is changed into air with the drying flow rate of 20ml/min, and reaction is carried out until the quality is constant as displayed by a computer;
(5) thus obtaining the weight loss curve of the whole sample, automatically calculating the contents of water and ash, and measuring the time for less than 30 min.
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| JPS6361137A (en) * | 1986-09-01 | 1988-03-17 | Nippon Komu Kk | Method and apparatus for testing flocculation property of coal slurry |
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