CN102826599B - Method for comparison and detection of calcined crystal seed activities - Google Patents
Method for comparison and detection of calcined crystal seed activities Download PDFInfo
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Abstract
The invention provides a method for comparison and detection of calcined crystal seed activities. The method for comparison of calcined crystal seed activities comprises the following steps of mixing calcined crystal seeds and water according to a preset volume ratio in a container having a preset height to obtain mixed slurry, carrying out sedimentation layering, and comparing activities of the calcined crystal seeds according to the height of a lower liquid layer, wherein the activities of the calcined crystal seeds are improved with increasing of the height of the lower liquid layer. The method for comparison and detection of calcined crystal seed activities has a low cost, simple and practical processes and strong operability, and is fast and accurate.
Description
Technical field
The present invention relates to the crystal seed Performance Detection technical field in Titanium White Production By Sulfuric Acid Process technique, more particularly, relate to detection method and the comparative approach of calcining seeds activity in a kind of Titanium White Production By Sulfuric Acid Process technique.
Background technology
At present, domestic 98% Producing Titanium Dioxide producer all adopts sulfuric acid process.In sulfuric acid process rutile type titanium white is produced, titanium liquid (titanyl sulfate) generally adopts automatic growing crystal species or titanyl sulfate plus seed nucleation, hydrolysis forms after metatitanic acid, after filtration, washing, add that calcining seeds, salt are processed and the operation such as calcining after form the rutile titanium white first product with certain pigment performance.Calcining seeds not only can promote product to change to rutile-type in the time of calcining, and can improve the pigment performance such as reducing power, form and aspect of product, and its shape of particle while improving calcining, makes round and smooth, the soft not easy-sintering of particle.
General, in domestic Producing Titanium Dioxide, calcining seeds obtains by operations such as the molten metatitanic acid of alkali, filtration, washing, peptizations, and calcining seeds essence is TiO 2 sol, is a kind of acid colloid that is.The activity of calcining seeds is in certain temperature range, promotes the ability that product transforms from anatase titanium dioxide to rutile-type, and the height of pigment performance, and the height of activity of crystal seed directly affects rutile content and pigment performance thereof in product.
The detection method that the active current domestic titanium white of calcining seeds enterprise takes is conventionally, the calcining seeds of preparation after filtration, the step such as oven dry, grinding, then measure rutile content wherein with X-ray diffractometer, rutile content quantity is active height.Because this detection method needs step more, generally need 3h just can obtain above testing result, and need to be equipped with special X-ray diffractometer, X-ray diffractometer belongs to large-scale precision instrument, needs to drop into hundreds of thousands at least, and fund up to a million is bought at most.Therefore, this detection method process is loaded down with trivial details, testing result is slower, and investment is larger.
Therefore, need a kind of method that cost is lower, simple and practical, detect fast and accurately calcining seeds activity badly.
Summary of the invention
The object of the invention is to solve the one or more problems in above shortcomings in prior art.
An aspect of of the present present invention provides a kind of comparative approach of calcining seeds activity.Described comparative approach comprises the following steps: according to predetermined volume ratio, calcining seeds and water are mixed in the container with predetermined altitude, to form mixed slurry; Sedimentation layering, and carry out the activity of comparison calcining seeds according to the height value of lower floor's liquid, described height value is higher, and the activity of calcining seeds is larger.
In an exemplary embodiment of the comparative approach of calcining seeds activity of the present invention, in described blend step, the volume ratio of calcining seeds and water can be 1.0～4.0.
In an exemplary embodiment of the comparative approach of calcining seeds activity of the present invention, described water can be the one in deionized water, desalted water, distilled water, and described electrical conductivity of water can be 0.1～2.0 μ s/cm.
In an exemplary embodiment of the comparative approach of calcining seeds activity of the present invention, the settling time of described precipitation step stratification step can be 1.5～2.5h.
A kind of detection method of calcining seeds activity is provided according to a further aspect in the invention.Described detection method comprises the following steps: according to predetermined volume ratio, calcining seeds and water are mixed in the container with predetermined altitude, to form mixed slurry, sedimentation layering is to draw the height value of lower floor's liquid; Use described sedimentation stratification step to draw respectively the height value of the corresponding lower floor of multiple different calcining seeds liquid; Measure the activity index of described multiple different calcining seeds; The activity index of each calcining seeds in described multiple different calcining seeds and the described height value of this calcining seeds are carried out corresponding one by one, form data look-up table, described data look-up table comprises the data group that multiple activity index by calcining seeds form with corresponding height value; Use described sedimentation stratification step to measure calcining seeds to be measured, to draw the height value of lower floor's liquid of described calcining seeds to be measured; In described data look-up table, find out the corresponding activity index of height value of lower floor's liquid of described calcining seeds to be measured.
In an exemplary embodiment of the detection method of calcining seeds activity of the present invention, described detection method also can comprise: the step that draws respectively the height value of the corresponding lower floor of multiple different calcining seeds liquid in described use sedimentation stratification step, each calcining seeds in described multiple different calcining seeds is all carried out repeatedly to described sedimentation stratification step, to draw multiple height values of the corresponding lower floor of each calcining seeds liquid, and calculate the arithmetic mean height value of described multiple height values; Then in the step of described formation data look-up table, the arithmetic mean height value of each calcining seeds is formed to data look-up table as the height value corresponding with the activity index of this calcining seeds.
In an exemplary embodiment of the detection method of calcining seeds activity of the present invention, in described sedimentation stratification step, can be 1.0～4.0 to mix according to volume ratio by calcining seeds and water.
In an exemplary embodiment of the detection method of calcining seeds activity of the present invention, described water can be the one in deionized water, desalted water, distilled water, and described electrical conductivity of water can be 0.1～2.0 μ s/cm.
In an exemplary embodiment of the detection method of calcining seeds activity of the present invention, the settling time of described precipitation step stratification step can be 1.5～2.5h.
Compared with prior art, the present invention have cost lower, simple and practical, quick and precisely, the advantage such as workable.
Embodiment
Hereinafter, describe comparison and the detection method of calcining seeds activity of the present invention in detail in connection with exemplary embodiment.
In one exemplary embodiment of the present invention, the comparative approach of calcining seeds activity comprises the following steps: according to predetermined volume ratio, calcining seeds and water are mixed in the container with predetermined altitude, to form mixed slurry; Sedimentation layering, and carry out the activity of comparison calcining seeds according to the height value of lower floor's liquid, described height value is higher, and the activity of calcining seeds is larger.In the present invention, described " lower floor's liquid " should be similar colloidal material strictly speaking, is not accustomed to " liquid " of call, but neither solid, and just in industry custom is called " lower floor's liquid "; Above described lower floor solution, be upper water solution.Here, in the case of the correlated condition such as volume ratio, container height of kind, calcining seeds and the water of the kind such as calcining seeds, water is definite, the activity of calcining seeds is corresponding with the height value of mixed slurry lower floor's liquid after layering in container, and described height value is larger, the activity of calcining seeds is larger.That is to say, can carry out according to said method the activity of more different calcining seeds.
In another exemplary embodiment of the present invention, the detection method of calcining seeds activity comprises the following steps: according to predetermined volume ratio, calcining seeds and water are mixed in the container with predetermined altitude, to form mixed slurry, sedimentation layering is to draw the height value of lower floor's liquid; Use described sedimentation stratification step to draw respectively the height value of the corresponding lower floor of multiple different calcining seeds liquid; Measure the activity index of described multiple different calcining seeds; The activity index of each calcining seeds in described multiple different calcining seeds and the described height value of this calcining seeds are carried out corresponding one by one, form data look-up table, described data look-up table comprises the data group that multiple activity index by calcining seeds form with corresponding height value; Use described sedimentation stratification step to measure calcining seeds to be measured, to draw the height value of lower floor's liquid of described calcining seeds to be measured; In described data look-up table, find out the corresponding activity index of height value of lower floor's liquid of described calcining seeds to be measured.
Preferably, in an exemplary embodiment of the detection method of calcining seeds activity of the present invention, described detection method also can comprise: the step that draws respectively the height value of the corresponding lower floor of multiple different calcining seeds liquid in described use sedimentation stratification step, each calcining seeds in described multiple different calcining seeds is all carried out repeatedly to described sedimentation stratification step, to draw multiple height values of the corresponding lower floor of each calcining seeds liquid, and calculate the arithmetic mean height value of described multiple height values; Then in the step of described formation data look-up table, the arithmetic mean height value of each calcining seeds is formed to data look-up table as the height value corresponding with the activity index of this calcining seeds.
Preferably, in the detection method of calcining seeds activity of the present invention or an exemplary embodiment of comparative approach, in the time of sedimentation layering, can be 1.0～4.0 to mix according to volume ratio by calcining seeds and water.
Preferably, in the detection method of calcining seeds activity of the present invention or an exemplary embodiment of comparative approach, described water can be the one in deionized water, desalted water, distilled water, pure water etc., and described electrical conductivity of water is 0.1～2.0 μ s/cm.
Preferably, in the detection method of calcining seeds activity of the present invention or an exemplary embodiment of comparative approach, the settling time of described precipitation step stratification step can be 1.5～2.5h.
Below, comparative approach of the present invention and detection method exemplary embodiment can realize according to following steps (using the graduated cylinder of 500ml as container).
Successively a certain amount of calcining seeds, water are joined in 500ml graduated cylinder, and the cumulative volume that makes calcining seeds and water is 500ml, calcining seeds and water are mixed to formation mixed slurry, after quiescent settling certain hour, read the height value of mixed slurry layering posterior end liquid.Then, judge the activity of calcining seeds by height value.
Particularly, this exemplary embodiment can comprise the following steps:
A, successively a certain amount of calcining seeds and water are joined in 500ml graduated cylinder.
Here, water can be the one in deionized water, desalted water, distilled water, and conductivity can be 0.1～2.0 μ s/cm; The cumulative volume of calcining seeds and water is 500ml, and the volume ratio of calcining seeds and water can be 1.0～4.0.
B, calcining seeds and water are mixed and formed after mixed slurry, quiescent settling is to the complete layering of mixed slurry; For example, the quiescent settling time can be 1.5～2.5h.
After C, quiescent settling 1.5～2.5h, observe the height value (also can be described as settling height value) of mixed slurry layering rear lower liquid.
In this exemplary embodiment, if settling height value is 250～370ml, adopt this kind of calcining seeds by conventional production method can obtain reducing power (Tcs) > 1780, brightness (Jasn) > 94.3, rutile content is more than 99% high quality titanium white product,, in this exemplary embodiment, the calcining seeds that settling height value is 250～370ml has good activity index.
Therefore, the present invention forms mixed slurry after can adding water dilution by calcining seeds, and the settling height after quiescent settling certain hour detects its activity, and have cost lower, simple and practical, quick and precisely, the advantage such as workable.Can be by, the present invention, compared with calcining seeds activity characterization method in the past, has obvious advantage, can better be used for and guiding production.
Enumerating concrete example is below further elaborated exemplary embodiment of the present invention.Example is only for the present invention is described, and not limits by any way the present invention.
In example below, characterize the activity of 6 calcining seeds by this inventive method, crystal seed numbering is respectively 1#, 2#, 3#, 4#, 5#, 6#.
Example 1
After the desalted water that is 1.0 μ s/cm by the conductivity of the 1# calcining seeds of 250ml and 250ml successively joins in 500ml graduated cylinder, stir and become the slurry mixing by stirring rod, after quiescent settling 2.0h, read the settling height of graduated cylinder lower liquid after mixed slurry layering, for 350ml, illustrate that activity of crystal seed is higher.
Example 2
After the deionized water that is 0.1 μ s/cm by the conductivity of the 2# calcining seeds of 125ml and 375ml successively joins in 500ml graduated cylinder, stir and become the slurry mixing by stirring rod, after quiescent settling 2.0h, read the settling height of graduated cylinder lower liquid after mixed slurry layering, for 370ml, illustrate that activity of crystal seed is higher.
Example 3
After the desalted water that is 2.0 μ s/cm by the conductivity of the 3# calcining seeds of 125ml and 375ml successively joins in 500ml graduated cylinder, stir and become the slurry mixing by stirring rod, after quiescent settling 2.5h, read the settling height of graduated cylinder lower liquid after mixed slurry layering, for 240ml, illustrate that activity of crystal seed is general.
Example 4
After the distilled water that is 1.5 μ s/cm by the conductivity of the 4# calcining seeds of 100ml and 400ml successively joins in 500ml graduated cylinder, stir and become the slurry mixing by stirring rod, after quiescent settling 2.5h, read the settling height of graduated cylinder lower liquid after mixed slurry layering, for 250ml, illustrate that activity of crystal seed is higher.
Example 5
After the desalted water that is 0.3 μ s/cm by the conductivity of the 5# calcining seeds of 100ml and 400ml successively joins in 500ml graduated cylinder, stir and become the slurry mixing by stirring rod, after quiescent settling 1.5h, read the settling height of graduated cylinder lower liquid after mixed slurry layering, for 190ml, illustrate that activity of crystal seed is poor.
Example 6
After the deionized water that is 0.78 μ s/cm by the conductivity of the 6# calcining seeds of 125ml and 375ml successively joins in 500ml graduated cylinder, stir and become the slurry mixing by stirring rod, after quiescent settling 2.0h, read the settling height of graduated cylinder lower liquid after mixed slurry layering, for 345ml, illustrate that activity of crystal seed is higher.
Respectively 1#～6# crystal seed is prepared to titanium white product testing.Calcining seeds is joined in two metatitanic acids after washing, after salt processing, calcining, form titanium white first product, carry out pigment performance and rutile content and test after being ground, it the results are shown in Table 1.
Table 1 calcining seeds is processed rear pigment performance and rutile content
| Calcining seeds | 1# crystal seed | 2# crystal seed | 3# crystal seed | 4# crystal seed | 5# crystal seed | 6# crystal seed |
| Reducing power (Tcs) | 1810 | 1790 | 1750 | 1820 | 1650 | 1800 |
| Brightness (Jasn) | 94.5 | 94.4 | 94.2 | 94.6 | 94.0 | 94.4 |
| Rutile content (R) % | 99 | 98 | 97 | 98 | 90 | 98.5 |
| Quality | High | High | Generally | High | Poor | High |
In sum, the present invention by measure calcining seeds after treatment the settling height value of mixed slurry quiescent settling judge the activity of corresponding calcining seeds, and the present invention has, and cost is lower, simple and practical, workable, the advantage such as quick and precisely.
Although described the present invention in conjunction with exemplary embodiment above, those of ordinary skills should be clear, in the case of not departing from the spirit and scope of claim, can carry out various modifications to above-described embodiment.
Claims (7)
1. a comparative approach for calcining seeds activity, is characterized in that, described comparative approach comprises the following steps:
According to predetermined volume ratio, calcining seeds and water are mixed in the container with predetermined altitude, to form mixed slurry;
Sedimentation layering, and carry out the activity of comparison calcining seeds according to the height value of lower floor's liquid, described height value is higher, and the activity of calcining seeds is larger,
In described blend step, the volume ratio of calcining seeds and water is 1.0～4.0.
2. the comparative approach of calcining seeds activity according to claim 1, is characterized in that, described water is the one in deionized water, desalted water, distilled water, and described electrical conductivity of water is 0.1～2.0 μ s/cm.
3. the comparative approach of calcining seeds activity according to claim 1, is characterized in that, the settling time of described precipitation step stratification step is 1.5～2.5h.
4. a detection method for calcining seeds activity, is characterized in that, described detection method comprises the following steps:
According to predetermined volume ratio, calcining seeds and water are mixed in the container with predetermined altitude, to form mixed slurry, sedimentation layering to be to draw the height value of lower floor's liquid, in described sedimentation stratification step, is 1.0～4.0 to mix calcining seeds and water according to volume ratio;
Use described sedimentation stratification step to draw respectively the height value of the corresponding lower floor of multiple different calcining seeds liquid;
Measure the activity index of described multiple different calcining seeds;
The activity index of each calcining seeds in described multiple different calcining seeds and the described height value of this calcining seeds are carried out corresponding one by one, form data look-up table, described data look-up table comprises the data group that multiple activity index by calcining seeds form with corresponding height value;
Use described sedimentation stratification step to measure calcining seeds to be measured, to draw the height value of lower floor's liquid of described calcining seeds to be measured;
In described data look-up table, find out the corresponding activity index of height value of lower floor's liquid of described calcining seeds to be measured.
5. the detection method of calcining seeds activity according to claim 4, it is characterized in that, described detection method also comprises: the step that draws respectively the height value of the corresponding lower floor of multiple different calcining seeds liquid in described use sedimentation stratification step, each calcining seeds in described multiple different calcining seeds is all carried out repeatedly to described sedimentation stratification step, to draw multiple height values of the corresponding lower floor of each calcining seeds liquid, and calculate the arithmetic mean height value of described multiple height values; Then in the step of described formation data look-up table, the arithmetic mean height value of each calcining seeds is formed to data look-up table as the height value corresponding with the activity index of this calcining seeds.
6. the detection method of calcining seeds activity according to claim 4, is characterized in that, described water is the one in deionized water, desalted water, distilled water, and described electrical conductivity of water is 0.1～2.0 μ s/cm.
7. the detection method of calcining seeds activity according to claim 4, is characterized in that, the settling time of described precipitation step stratification step is 1.5～2.5h.
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| CN106745233A (en) * | 2016-11-24 | 2017-05-31 | 攀枝花市钛都化工有限公司 | For the preparation method of the calcining seeds of rutile titanium white powder production |
| CN108002437A (en) * | 2017-11-15 | 2018-05-08 | 南京钛白化工有限责任公司 | A kind of preparation of sulfate process titanium dioxide calcining seeds and detection method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4829031A (en) * | 1986-08-01 | 1989-05-09 | Research Corporation | Method of preparing ceramic compositions at lower sintering temperatures |
| CN101311120A (en) * | 2008-05-05 | 2008-11-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of rutile type calcining seeds with high activity and high stability |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4829031A (en) * | 1986-08-01 | 1989-05-09 | Research Corporation | Method of preparing ceramic compositions at lower sintering temperatures |
| CN101311120A (en) * | 2008-05-05 | 2008-11-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of rutile type calcining seeds with high activity and high stability |
Non-Patent Citations (2)
| Title |
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| 纳米二氧化钛粉体的制备及其在水相介质中的分散性研究;龙海云;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20071123(第6期);第17页第2.3.3节，第20-21页第2.5.2节 * |
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