CN105334134A - Method for determining residence time of titanium concentrate in high-temperature fluidization reactor - Google Patents
Method for determining residence time of titanium concentrate in high-temperature fluidization reactor Download PDFInfo
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- CN105334134A CN105334134A CN201510702154.XA CN201510702154A CN105334134A CN 105334134 A CN105334134 A CN 105334134A CN 201510702154 A CN201510702154 A CN 201510702154A CN 105334134 A CN105334134 A CN 105334134A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The invention belongs to the field of chemical engineering, and particularly relates to a method for determining the residence time of titanium concentrate in a high-temperature fluidization reactor. The technical problem that due to the fact that an ordinary tracer agent cannot play a role at high temperature, the residence time of materials in a reactor is difficult to determine is solved. In order to solve the technical problem, the method for determining the residence time of the titanium concentrate in the high-temperature fluidization reactor is provided. The method comprises the following steps that 1, a tracer agent is added to the titanium concentrate at a constant speed in the process that the titanium concentrate is added to the high-temperature fluidization reactor; 2, after the titanium concentrate is completely reacted, the tracer agent is sorted and recycled through a magnetic extractor to be weighed in real time; 3, the average residence time of the titanium concentrate is calculated according to the corresponding relation of the real-time weighed mass of the tracer agent and the time. The method for determining the residence time of the titanium concentrate in the high-temperature fluidization reactor is easy, rapid and convenient to operate, good in repeatability, accurate in determination, better in representativeness, less in equipment investment, low in operating cost and very suitable for large-scale industrial application.
Description
Technical field
The invention belongs to field of chemical engineering, be specifically related to the assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor.
Background technology
Fluidized-bed reactor because of its there is good mixing, heat transfer, mass-transfer efficiency are high, dynamic conditions is good, and the advantages such as easy are amplified in industrialization, have been widely used in the numerous areas such as chemical industry, the energy, light industry, metallurgy, material, medicine, food and environmental protection.But, fluid and particle are interactional in a fluidized bed reactor, the displacement potential of each particle must cause the change of this some place fluid velocity, this change has influence on again the displacement of particle, and different fluid speed causes movement of particles pattern and track to have bigger difference, therefore, Particle Behavior is not simply caused by Hydrodynamic turbulence in even loose formula flow field, Particle Behavior track is complicated, and change is large, poor reproducibility.To system complicated like this, operational factor determination difficulty is large, research difficulty, and therefore fluidizing reactor operational factor adopts average concept to substitute individual research substantially.
The residence time leaves the experienced time from entering into when referring to the process equipment of material by continued operation.In material, each particle has the corresponding residence time, namely there is residence time destribution (residencetimedistribution, RTD).RTD is the basic parameter of characterization construction equipment performance, Flow of Goods and Materials and the other problems such as mixing, Chemical Kinetics, heat and mass relevant with flowing in main equipment.
Panzhihua ilmenite concentrate because of its impurity content high, acid-soluble good, prepare in synthetic rutile technique must carry out high temperature Strong oxdiative to it, crystalline structure that reduction pretreatment changes its titaniferous thing phase, react with hydrochloric acid in effective restraint leaching process, dissolving and hydrolysis cause grain refine, improve wherein impurity element reactivity simultaneously, promote impurity element clearance, improve synthetic rutile product quality.For ilmenite concentrate high-temperature heat treatment process, the crystalline structure of the RTD of ilmenite concentrate in fluidizing reactor and this process transforms closely related, and then impact is in product quality.
Patent CN101839859B discloses a kind of device for testing residence time distribution (RTD) of material, the light beam launched by excitation source incides on tested material through semi-transparent semi-reflecting lens, tracer agent in tested material is subject to exciting rear emitting fluorescence, described fluorescence is transferred to fluorescent probe after semi-transparent semi-reflecting lens, analyzed by signal processing unit, calculate residence time of material distribution.Main equipment mainly comprises logical light pipe, optical window, fluorescent probe, signal processing unit, excitation source, semi-transparent semi-reflecting lens and light source power supply unit etc.Major advantage: excitation beam and fluorescence do not need and coupling fiber in outgoing process, can significantly reduce coupling loss and cost, and light path arrangement is compact, proving installation small volume.Device for testing residence time distribution (RTD) of material is only electrically connected with signal processing unit and light source power supply unit, extremely easy to use, and conveniently can isolate the high temperature and high pressure environment of tested material.Shortcoming: complex structure, stability is not high, is subject to reactor high temperature environmental impact, real time on-line monitoring, and tracer agent running orbit in reactor is complicated, needs through powerful calculating and professional software process, and industrialization uses cost higher.
In patent 200410025407.6 and patent 200710179497.8, to the concentration determination of tracer mainly based on principles such as radioactivity, ultrasonic reflections, optical reflection, electric conductivity, magnetic, near infrared absorption, adopt MnO
2, La
2o
3, filler, carbon black, TiO
2, KNO
3, NaCl, iron powder, the tracer of different nature such as colored dyes.
Patent CN201010510265.8 discloses the assay method of a kind of tobacco residence time destribution in process equipment, comprises the following steps: a, in tobacco, select a certain usual ingredients as tracer, meets accuracy testing requirement; B, tracer is added the equipment entrance streams of steady operation with a certain tracing method, the response simultaneously detecting its concentration changes with time in outlet with certain hour interval obtains residence time destribution (RTD) function; C, by this function with suitable flow model carry out nonlinear fitting can obtain this function model equation and try to achieve material mean residence time and at equipment axis degree of mixing upwards.The major advantage of this invention is: 1. use a certain usual component in tobacco to measure the RTD of tobacco in process equipment as tracer, and the test duration is short, coverage is little, detection method accuracy is high, little on product quality impact, can not constitute a threat to the safety of consumer; 2. the method can be predicted, optimizes and control at quality of item.Shortcoming is strongly professional, narrow application range.
Panzhihua ilmenite concentrate high temperature Strong oxdiative reduction pretreatment, is intended to change titaniferous phase structure, the therefore conversion ratio of the direct ectocrine phase structure of ilmenite concentrate mean residence time in the reactor in ilmenite concentrate.Keep about 1000 DEG C high temperature in simultaneous reactions device, common tracer agent cannot play a role, and cause residence time of material in reactor to measure difficulty large, existing method of testing can not be applied to this system substantially.
Summary of the invention
The technical problem to be solved in the present invention is that common tracer agent cannot play a role, and causes residence time of material in reactor to measure difficulty large.
The scheme that the present invention solves the problems of the technologies described above is to provide the assay method of the ilmenite concentrate residence time in a kind of high-temperature fluidizedization reactor, comprises the following steps:
A, to stablize at ilmenite concentrate join high-temperature fluidizedization reactor process in, tracer agent is at the uniform velocity joined in ilmenite concentrate;
B, after the reaction of ilmenite concentrate in high-temperature fluidizedization reactor terminates, reclaim tracer agent weighing in real time in the discharging opening magnetic separator sorting of high-temperature fluidizedization reactor, when the tracer agent recovery reaches more than 95%, recovery completes;
C, the quality of weighing in real time according to tracer agent and the corresponding relation of time, calculate the mean residence time of ilmenite concentrate.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, the tracer agent described in step a is iron ore concentrate.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, add that total amount is ilmenite concentrate quality 5% ~ 15% of tracer agent described in step a.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, the joining day of tracer agent described in step a is 20 ~ 40min.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, the formula calculating ilmenite concentrate mean residence time described in step c is:
t
ifor the time of weighing in removal process, A
ifor t in removal process
ito weigh the Iron Concentrate Quality obtained.
The assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor provided by the invention, utilize iron ore concentrate as the mean residence time of tracer test reaction mass, accuracy is high, can not destroy the continous-stable of system cloud gray model, can not impact system operational parameters.Meanwhile, due to tracer agent performance and reactant institute containing element basically identical, also can not pollute product even if slight trace agent enters system.Method provided by the invention is simple to operation, convenient, and favorable reproducibility measures accurately, have good representativeness, and equipment investment is few, operating cost is low, is very applicable to large-scale industrial application.
Embodiment
The assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor, comprises the following steps:
A, join at ilmenite concentrate in the process of high-temperature fluidizedization reactor, tracer agent is at the uniform velocity joined in ilmenite concentrate;
B, after the reaction of ilmenite concentrate in high-temperature fluidizedization reactor terminates, reclaim tracer agent weighing in real time in the discharging opening magnetic separator sorting of high-temperature fluidizedization reactor, when the tracer agent recovery reaches more than 95%, recovery completes;
C, the quality of weighing in real time according to tracer agent and the corresponding relation of time, calculate the mean residence time of ilmenite concentrate.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, the tracer agent described in step a is iron ore concentrate.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, add that total amount is ilmenite concentrate quality 5% ~ 15% of tracer agent described in step a.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, the joining day of tracer agent described in step a is 20 ~ 40min.
In above-mentioned high-temperature fluidizedization reactor the ilmenite concentrate residence time assay method in, the formula calculating ilmenite concentrate mean residence time described in step c is:
t
ifor the time of weighing in removal process, A
ifor t in removal process
ito weigh the Iron Concentrate Quality obtained.Because the stroke of tracer agent and ilmenite concentrate is completely the same, so the quality can weighed in real time according to tracer agent and the corresponding relation of time, calculate the mean residence time of ilmenite concentrate.
Ilmenite concentrate, through the pre-service of high temperature Strong oxdiative, changes ilmenite concentrate crystalline structure, and effectively preventing reacts with hydrochloric acid in its leaching process causes the refinement of synthetic rutile product.Strengthen ilmenite concentrate impurity element reactivity by the process of high temperature Strong oxdiative simultaneously, improve impurity element clearance, obtain high-quality synthetic rutile product.Pre-service uses gas-solid fluidization reaction pattern, select gas-solid fluidized bed (a kind of high-temperature fluidizedization reactor), temperature of reaction 900 ~ 1100 DEG C, ilmenite concentrate residence time length in fluidized bed directly affects crystalline structure conversion ratio and impurity element clearance, affecting synthetic rutile product quality, is one of pretreatment process major control index.By analyzing the performance of ilmenite concentrate and iron ore concentrate, their essential elements are basically identical, even if the impurity element in iron ore concentrate is mixed in ilmenite concentrate, its impurity element, all by rear operation process, can not impact synthetic rutile product quality.But Fe, Ti content of ilmenite concentrate and iron ore concentrate difference is larger, mineral phase structure and crystalline structure are all different, therefore two kinds of mineral differ greatly than magnetizing system, magnetic plant is utilized after high-temperature fluidizedization reactor, according to specific susceptibility difference after two kinds of mineral pyroprocessing, sub-elect iron ore concentrate by adjustment magnetic field intensity, therefore the present invention selects iron ore concentrate as the tracer agent of ilmenite concentrate high-temperature roasting.
Embodiment 1
A, join in the process of high-temperature fluidizedization reactor at ilmenite concentrate 1500kg/h, 30min at the uniform velocity adds 60kg iron ore concentrate, to have fed intake as time zero.
B, after the reaction of ilmenite concentrate in high-temperature fluidizedization reactor terminates, tracer agent weighing 1 time for every 1 minute is reclaimed, till the tracer agent recovery to reach in more than 95% ilmenite concentrate substantially without iron ore concentrate in the discharging opening magnetic separator sorting of high-temperature fluidizedization reactor.
Iron Concentrate Quality A is obtained in c, removal process
iwith time t
ias shown in table 1.
Iron Concentrate Quality and time is obtained in table 1 removal process
By calculating, it is 98.98% that iron ore concentrate adds yield, passes through formula:
calculating ilmenite concentrate mean residence time is in the reactor 88.5min.
Method provided by the invention is simple to operation, convenient, and favorable reproducibility measures accurately.
Claims (5)
1. the assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor, comprises the following steps:
A, join at ilmenite concentrate in the process of high-temperature fluidizedization reactor, tracer agent is at the uniform velocity joined in ilmenite concentrate;
B, after the reaction of ilmenite concentrate in high-temperature fluidizedization reactor terminates, reclaim tracer agent weighing in real time in the discharging opening magnetic separator sorting of high-temperature fluidizedization reactor, when the tracer agent recovery reaches more than 95%, recovery completes;
C, the quality of weighing in real time according to tracer agent and the corresponding relation of time, calculate the mean residence time of ilmenite concentrate.
2. the assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor according to claim 1, is characterized in that: the tracer agent described in step a is iron ore concentrate.
3. the assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor according to claim 1, is characterized in that: add that total amount is ilmenite concentrate quality 5% ~ 15% of tracer agent described in step a.
4. the assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor according to claim 1, is characterized in that: the joining day of tracer agent described in step a is 20 ~ 40min.
5. the assay method of the ilmenite concentrate residence time in high-temperature fluidizedization reactor according to claim 1, is characterized in that: the formula calculating ilmenite concentrate mean residence time described in step c is:
t
ifor the time of weighing in removal process, A
ifor t in removal process
ito weigh the Iron Concentrate Quality obtained.
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|---|---|---|---|
| CN201510702154.XA CN105334134A (en) | 2015-10-26 | 2015-10-26 | Method for determining residence time of titanium concentrate in high-temperature fluidization reactor |
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|---|---|---|---|
| CN201510702154.XA CN105334134A (en) | 2015-10-26 | 2015-10-26 | Method for determining residence time of titanium concentrate in high-temperature fluidization reactor |
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| CN105334134A true CN105334134A (en) | 2016-02-17 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5062713A (en) * | 1989-09-06 | 1991-11-05 | The Dow Company | Method for determining the residence time distribution of a polymer extruder |
| JP2001191048A (en) * | 2000-01-13 | 2001-07-17 | Osaka Gas Co Ltd | Tracer for heat treatment furnace and method for measuring stagnation time using the same |
| CN1595113A (en) * | 2004-06-17 | 2005-03-16 | 浙江大学 | Polymer stay time distribution on-line measurement method and system |
| CN101183051A (en) * | 2007-12-14 | 2008-05-21 | 北京化工大学 | Material detention period and distributing on-line measurement system and method |
| CN101793854A (en) * | 2010-02-10 | 2010-08-04 | 中北大学 | Device and method for online measurement of residence time distribution of rotating packed bed |
| CN101839859A (en) * | 2010-05-20 | 2010-09-22 | 杭州远方光电信息有限公司 | Device for testing residence time distribution (RTD) of material |
-
2015
- 2015-10-26 CN CN201510702154.XA patent/CN105334134A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5062713A (en) * | 1989-09-06 | 1991-11-05 | The Dow Company | Method for determining the residence time distribution of a polymer extruder |
| JP2001191048A (en) * | 2000-01-13 | 2001-07-17 | Osaka Gas Co Ltd | Tracer for heat treatment furnace and method for measuring stagnation time using the same |
| CN1595113A (en) * | 2004-06-17 | 2005-03-16 | 浙江大学 | Polymer stay time distribution on-line measurement method and system |
| CN101183051A (en) * | 2007-12-14 | 2008-05-21 | 北京化工大学 | Material detention period and distributing on-line measurement system and method |
| CN101793854A (en) * | 2010-02-10 | 2010-08-04 | 中北大学 | Device and method for online measurement of residence time distribution of rotating packed bed |
| CN101839859A (en) * | 2010-05-20 | 2010-09-22 | 杭州远方光电信息有限公司 | Device for testing residence time distribution (RTD) of material |
Non-Patent Citations (1)
| Title |
|---|
| 陈德明: ""钛精矿颗粒在内构件流化床内停留时间特性的研究"", 《钢铁钒钛》 * |
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Application publication date: 20160217 |