CN107585779B - A kind of preparation method containing chrome-magnesite - Google Patents
A kind of preparation method containing chrome-magnesite Download PDFInfo
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- CN107585779B CN107585779B CN201710956812.7A CN201710956812A CN107585779B CN 107585779 B CN107585779 B CN 107585779B CN 201710956812 A CN201710956812 A CN 201710956812A CN 107585779 B CN107585779 B CN 107585779B
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Abstract
The invention discloses a preparation methods containing chrome-magnesite, by lye and contain Cr3+Solion, which synchronizes, to be added dropwise in the aqueous solution containing magnesium oxide source, and the heavy chromium reaction of magnesium oxide source grain surface is carried out；It is separated by solid-liquid separation after the reaction was completed, obtains presoma containing chrome-magnesite；The presoma first carries out one-step calcination at 900 ± 50 DEG C, carries out two step calcinings at 1600 ± 50 DEG C again after tabletting, obtains containing chrome-magnesite.The present inventor passes through a large number of experiments the study found that in heavy chromium reaction process, lye is added into solution containing magnesium oxide source and containing Cr by synchronous3+Solion can unexpectedly increase the probability that chromium hydroxide is nucleated in a manner of heterogeneous nucleation, Cr3+Ion and OH‑It enters to uniform ion in the lattice of magnesium oxide source surface microstructure, it avoids the chromium hydroxide to be formed and falls off and separate from magnesium oxide source surface, and greatly improve that chromium hydroxide is uniformly dispersed in presoma, and then (mixture of chrome green and magnesia) containing chrome-magnesite being had excellent performance.
Description
Technical field
The invention belongs to magnesia preparation fields, and in particular to a kind of preparation method containing chrome-magnesite.
Background technique
Magnesia refers to the material with MgO for main object phase, is being commonly called as magnesia, white or faint yellow blocks of solid,
Have the characteristics that refractoriness is high, alkali resistance slag penetrating power is strong, is a kind of important raw material for refractory, is widely used in metallurgy
Oxygen coverter used in the lining of industry high-temperature service, especially smelting iron and steel, electric furnace, ladle etc. are not only able to effectively resist
The erosion of high scum, moreover it is possible to promote molten steel purity to a certain extent.Currently, industrial high-temperature service mainly use it is magnesia multiple
Condensation material, such as by the composite material of magnesia and chromite.
Magnesia and chromite are combined magnesian-chrome efractoy, the method to promote lining service life, 100
It has just been suggested many years ago.Magnesium chromium matter composite material, it is bright in the ability for resisting Temperature cycling cataclysm, alkaline scouring
It is aobvious to be better than its single raw material.Micro chromated oxide or chromium are added in magnesia refractories, in addition to using heterogeneity,
The characteristics such as bulk effect promote the quality of refractory product, and chromated oxide still can play it in traditional magnesium chromium in these materials
The effect of destruction is resisted in refractory material, that is, is resisted chemistry and melted down and thermal shock resistance damage, although effect is necessarily not so good as traditional material,
But in terms of cost and environmental protection, it is better than traditional material.
Some preparation methods containing chrome-magnesite are reported in the prior art, such as: the Layden discovery of PSU adds in MgO
Add a small amount of chromium to help to promote magnesia, and calcine at 1255 DEG C, improves sintered density[1]。
Li Jing's victory of Wuhan University Of Technology etc.[2]By way of ball milling, by Cr2O3It mixes in magnesia, passes through ball press technique
The presoma for mixing chromium is formed, the magnesium aluminate spinel phase for obtaining mixing chromium is finally calcined at 1650 DEG C.
At normal temperature, chromium hydroxide is prepared using chromic salts and ammonium hydroxide and be generally obtained crystalline products, the reason is that weak base can
To slowly release OH-ion, it is more advantageous to the growth of chromium hydroxide crystal grain.When there are chromium ions in light calcined magnesia ore pulp
When, when appropriate alkaline precipitant to certain degree of supersaturation is added, chromium hydroxide starts to be nucleated.Due to chromium hydroxide solubility product Ksp
It is extremely low, it is easy to precipitate in a manner of homogeneous nucleation, the chromium hydroxide partial size which is formed is smaller, is easy and larger light calcined magnesia
Particle generates sedimentation separation.Since light-burned powder particles are thicker, particle diameter distribution is uneven, and control condition increases chromium hydroxide partial size
It is unanimously difficult to as light-burned powder particles greatly.
[1]G.K.LAYDEN and M.C.McQUARRIE.Effect of Minor Additions on
Sintering of MgO [J] .Am.Ceram.Soc., 1959 (42): 89-92.
[2] L.Jingjie, Z.Huizhong, Z.Pengda, C.Jiangtao, M.Songlin, and
L.Yongfeng.Effects of Cr2O3addition on property improvement of magnesia-spinel
Refractories used in RH snorkel [J] .Ceram.Int., 2016 (42): 18579-18584.
Summary of the invention
To solve the shortcomings of the prior art, current inventor provides a kind of preparation methods containing chrome-magnesite, it is intended to make
It must be more evenly distributed, performance more preferably contains chrome-magnesite.
A kind of preparation method containing chrome-magnesite by lye and contains Cr3+Solion, which synchronizes, is added dropwise to the water containing magnesium oxide source
In solution, the heavy chromium reaction of magnesium oxide source grain surface is carried out；It is separated by solid-liquid separation after the reaction was completed, obtains presoma containing chrome-magnesite；
The presoma containing chrome-magnesite first carries out one-step calcination at 900 ± 50 DEG C；Two step calcinings are carried out at 1600 ± 50 DEG C again,
It obtains containing chrome-magnesite.
The present inventor is had found by numerous studies, in heavy chromium reaction process, by synchronous into solution containing magnesium oxide source
Add lye and containing Cr3+Solution can unexpectedly increase the probability of chromium hydroxide forming core in a manner of heterogeneous nucleation；Cr3+Ion
With OH-ion evenly into the lattice of magnesium oxide source surface microstructure, the chromium hydroxide to be formed is avoided from magnesium oxide source
Surface falls off and separates, and greatly improves that chromium hydroxide is uniformly dispersed in presoma, and then had excellent performance
Containing chrome-magnesite (mixture of chrome green and magnesia).
The method of the present invention is realized chromium hydroxide and is deposited in light calcined magnesia lattice surface in a manner of heterogeneous nucleation, more
Easily obtain ingredient uniform precursor；By subsequent two steps calcination process, finally realizes and uniformly divide in magnesium oxide source lattice
Cloth chrome green；Compared to existing conventional use chrome green and magnesia by physical admixture, the present invention is obtained
The physical and chemical indexes uniformity containing chrome-magnesite arrived is more preferable.
In the present invention, the lye is the mixture of the aqueous solution of alkali metal hydroxide, ammonium hydroxide or both.
The alkali metal hydroxide is, for example, sodium hydroxide, potassium hydroxide etc..
Preferably, the pH of the lye is 9~13.
The concentration of the alkali does not specially require, preferably 1~2mol/L.
In the present invention, contain Cr3+Solution is the aqueous solution of chromic salt.
The chromic salt is preferably Cr3+Water soluble salt；Such as nitrate.
Preferably, Cr3+Concentration be 0.2~0.4mol/L.
In the present invention, the solution containing magnesium oxide source is the aqueous solution for being dispersed with magnesium oxide source.
The magnesium oxide source is common magnesite light burnt powder, other magnesium oxide materials such as common caustic-calcined magnesite.
In the solution containing magnesium oxide source, solid content is 20~45wt%；Further preferably 35~45wt%；It is optimal
It is selected as 45wt%.
The inventors discovered that the temperature of heavy chromium reaction process has larger impact to uniformity of heavy chromium product etc..
Surface is studied, the temperature of heavy chromium reaction process is preferably 30~75 DEG C.At such a temperature, coordinated is in this for control
Concentration of lye, the Cr of invention3+The solid content and synchronous dosing method of concentration, the aqueous solution containing magnesium oxide source, make magnesium hydroxide chromium
It is uniformly deposited in the lattice surface of magnesium oxide source, can help to the chromium hydroxide and magnesium oxide source phase that further avoid precipitating
Separation, facilitates the dispersing uniformity for further promoting the chromium of obtained presoma.
Further preferably, the temperature of heavy chromium reaction process is preferably 40~60 DEG C；Most preferably 45 DEG C.
Preferably, the dosage containing Cr (III) solution be make finally to synthesize obtain containing chromium in chrome-magnesite (with Cr2O3
Meter) weight percent be 0.2~0.4%.In actual mechanical process, it can control and contain Cr3+Chromic salt and magnesia in solution
Weight ratio between source is 1: 15~25.
Research controls it is also shown that under the reaction temperature, concentration in suitable stirring rate and reaction time
Under, facilitate the uniformity for further promoting the chromium of obtained presoma.
Preferably, the mixing speed of heavy chromium reaction process is 200~650r/min.
Preferably, the time of heavy chromium reaction is 0.5~2h.
Using a step, two step calcine technologies, facilitates obtained uniformity and preferably contain chrome-magnesite.
Existing equipment can be used in one step, two step calcination process, and the atmosphere of calcination process is air atmosphere.
In the present invention, the time of one-step calcination is 1~2h.
The time of two steps calcining is 3~4h.
Preferably, the preparation method, the product of a section calcining carries out two steps again after compressing tablet process and forges
It burns.Through research, the inventor has found that after cooling to one-step calcination product, then through compressing tablet process, will then suppress obtained piece
Material carries out two step calcinings again；The bulk density containing chrome-magnesite can be improved in compressing tablet process.
One-step calcination processing, helps to remove the combination water containing in chrome-magnesite, additionally aids subsequent compressing tablet process.
Further preferably, again through the compressing tablet process after the one-step calcination product and adhesive mix.The present invention
Research also found, originally by tabletting after one-step calcination product and adhesive mixing；Facilitate what further promotion obtained
Performance containing chrome-magnesite.
The adhesive can be used it is existing it is conventional can be by the material of a section calcining product adhesive.
Preferably, the adhesive is at least one of PVA, sodium carboxymethylcellulose, chitosan.PVA viscosity
The stable solvent resistance of larger and performance is strong, and the performance of finally obtained material is further promoted.
Preferably, the additive amount of the adhesive is 1~3wt% of a section calcining products weight.It is preferred at this
Under additive amount, the use of adhesive will not influence the finally obtained properties of product containing chrome-magnesite, and in the lower additive amount
Under, it remains to play good adhesive effect.
The technological parameter of tableting processes does not specially require.The material compacting that existing method is blended with adhesive can be used
At sheet material；Such as 1~3mins of PVA tabletting is added under 25~30Mpa pressure, sheet material is made.
The present invention is using cheap light burnt powder as bottom material, using chromic salt as auxiliary material, probes into production predecessor containing chrome-magnesite
New process.And the calcium impurities of product are removed aquation and by way of additive is added, finally prepared into two steps annealing method
Product contain chrome-magnesite.
A kind of preferred preparation method of the present invention, comprising the following steps:
Step (1): sodium hydroxide is configured to 2mol/L solution (lye).
Pure chromic nitrate will be analyzed with deionized water and is configured to the solution of 0.3167mol/L (containing Cr (III) solution).
Step (2): taking appropriate light burnt powder to be dispersed in water, and obtains the magnesia suspension that solid content is 20~45wt%；With
It is synchronized in backward magnesia suspension and adds the chromium salt solution and sodium hydroxide solution；In 30~75 DEG C, 200~650r/
(heavy chromium reaction) 0.5~2h is stirred to react under min.
Step (3): predecessor will be obtained after the reaction solution filtering of step (2), drying.
Step (4): predecessor is placed at 900 DEG C and calcines 1h.
Step (5): being added a small amount of PVA adhesive after the calcined product of step (4) is ground, tabletted with tablet press machine
Tablet is finally placed in high-temperature calcination 3h at 1600 DEG C, finished product is obtained after cooling containing chrome-magnesite by (sheet material).
The invention also includes use to contain chrome-magnesite made from the preparation method；Described contains in chrome-magnesite, Cr2O3Contain
Amount is 0.2%~0.4%, content of MgO 98.5%.
In the present invention, in preparation process, there can be the white thin mud of doubtful carbonate, and light burnt powder ore pulp is in reaction process
There is more foam on middle surface, these existing in-situ depositions for all largely influencing chromium hydroxide.By the study found that by lye
With chromium source synchronize add, facilitate promoted chromium hydroxide secondary nucleation probability, facilitate the presoma being evenly distributed, then
The secondary clacining technique for cooperating the application can make chromium distribution more evenly, also make product itself more beautiful.
Beneficial effect
In the present invention, by the preparation method, chromium hydroxide can be made mainly to be deposited on oxygen in a manner of heterogeneous nucleation
Change in the lattice surface of magnesium source；Facilitate the uniformity for the material that promotion obtains.
The present invention obtained presoma is originally also subjected to tabletting or is mixed with the adhesive after again through pressing
Piece processing；The sheet material that compressing tablet process is obtained carries out the two step calcination processings again, helps further to be made and has excellent performance
Contain chrome-magnesite.
Detailed description of the invention
Fig. 1 is No. 6 SEM figures for testing product of the obtained presoma under 900 DEG C of calcinings；
Fig. 2 is the SEM figure of product of No. 6 sheet materials tested after obtained tabletting under 1600 DEG C of calcinings.
Particular content
Magnesite light burnt powder technical grade Gansu Jin Mao Sociedad De Desarrollo Minero Limitada "Sodemi Ltda" provides.
Embodiment 1
Step (1): sodium hydroxide is configured to 2mol/L solution (lye).
Pure chromic nitrate will be analyzed and is configured to the solution of 0.3167mol/L with deionized water (containing Cr3+Solution；Chromic salts is molten
Liquid).
Step (2): taking appropriate light burnt powder to be scattered in gauge water, obtains the light burnt powder solution that solid content is 20~45wt%；
Chromium salt solution (5mL) and sodium hydroxide solution (5mL) is added dropwise into light burnt powder solution simultaneously.Keep the two identical
Rate of addition stirs under 200~650r/min and carries out heavy chromium reaction at 30~75 DEG C；The mine obtained after 0.5~2h of reaction
Slurry filtered, dry after obtain predecessor containing chrome-magnesite.
Step (3): predecessor being placed at 900 DEG C and calcines 1h, be added after cooling calcined product weight 2.5% (i.e.
Be added and initial magnesite light burnt powder mass ratio 1: 40) PVA grinds in 15min and is pressed into 30Mpa pressure as adhesive
Piece, and pressure maintaining 2min, tabletting to tablet is stablized repeatedly.
Step (4): the tablet that step (3) obtains finally is placed in high-temperature calcination 3h at 1600 DEG C, obtains finished product after cooling
Containing chrome-magnesite.
The present inventor sieves the solid content of step step (2), speed of agitator, heavy chromium reaction temperature and reaction time
It looks into；Concrete operations and parameter are shown in Table 1:
Predecessor is placed in drying box at 110 DEG C and dries 2h, takes the powder about 1g after drying in 200mL beaker,
Add 15mL water to disperse powder, is then added dropwise by concentrated nitric acid through isometric water-reducible solution (nitric acid solution) 10mL, after shaking up
Solid powder is suitably heated to all to dissolve.After sample solution is cooling, transfer them to constant volume in 100mL volumetric flask, be made to
Sample measuring liquid, and titrated using EDTA titration.
The filter cake of predecessor containing chrome-magnesite bottom chrome content as main indicator, filter cake surface layer chrome content as secondary index,
And its calcium ions and magnesium ions content is measured respectively.It will contain after chrome-magnesite is sintered into, bulk density also as index is considered, probes into technique
Influence of the condition to magnesia bulk density.Filter cake component list sees attached list 2, the filter cake (presoma) that 16 groups of table 1 are tested at
Divide table 2.
Table 2
K when using chromium uniformity as index, about each leveliThe R value of value and each factor, is shown in Table 2, wherein A is
Time factor, B are temperature factor, and C is solid content factor, and D is mixing speed factor, and each factor level value presses numerical value from small to large
Distribute code name 1,2,3,4；Analysis the results are shown in Table 3.
Table 3
Table 3 is horizontalValue and factor R value table
Research shows that relatively being closed the chromium content of bottom filter cake as the main indicator for measuring magnesia chromium distributing homogeneity
Reason.AndThe average value of each sample bottom filter cake chrome content, is maximized in each factor as under same level, can determine
One theoretical optimum combination, R value are very poor, the bigger influence for representing the factor to product quality of R value of each level in each factor
It is bigger.
Therefore the importance ranking of factor are as follows: temperature > solid content > reaction time > mixing speed.It therefore follows that most
Excellent group is combined into No. 6 groups, i.e. 60 DEG C of reaction temperature, 45% solid content, stirring 1h, mixing speed 500r/min.
The influence to the crystal habit containing chrome-magnesite is calcined for research different temperatures, is most preferably tested using No. 6 groups that table 1 is mentioned
Condition, attached drawing 1 are the form containing chrome-magnesite of 900 DEG C of calcinings, and attached drawing 2 is the magnesia form of 1600 DEG C of calcinings.
It can be seen that 900 DEG C of magnesia surface is more smooth and powder dispersity is preferable, bulk density is relatively small, may
Cr when as the temperature rises to 1600 DEG C2O3Middle Cr3+Gradually it is dissolved into the crystal structure for having broken original MgO in crystal grain
More lattice energies are produced, more stable structure, and Cr are formed3+It can promote long ambassador's volume of crystal as the temperature rises
Density increases, and keeps powder surface more coarse.
Embodiment 2
It is compared with embodiment 1, tests presoma obtained using No. 6, the PVA with 0%, 1%, 2% and 3% is carried out respectively
Tabletting, then carry out subsequent calcination processing.Different PVA tablettings is added, the performance data of obtained product is shown in Table 4:
Table 4
To be known by table 4, the additional amount of PVA has bulk density containing chrome-magnesite and influences, with the increase of PVA additional amount,
Experiment is too small with tablet press machine pressure, forms predecessor containing chrome-magnesite so needing to add appropriate binder, but adds bonding
Agent can be such that the bulk density containing chrome-magnesite declines, and see Table 4 for details this is because binder density is lower, containing necessarily accounting in chrome-magnesite
According to certain volume vacancy, although binder becomes gas during the sintering process, still can be left a void in containing chrome-magnesite.
In addition, the present invention is also attempted presoma (No. 6 experiments of embodiment 1 obtain) direct tablet compressing, then carries out two steps and forge
It burns, containing there is mass crystallization water in chrome-magnesite, the calcining of presoma direct tablet compressing can generate many gaps, influence the densification of material for discovery
Degree, causes fire resistance to decline, and effect is big not as good as the progress two steps calcining bulk density of tabletting again is first calcined.
In technology development process, lye or chromic salts are successively added into magnesium oxide source solution (either to chromium ion solution
Middle dropwise addition lye, or chromium ion solution is added dropwise into lye), distributing homogeneity of the finally obtained chromium in magnesia is paid no attention to
Think；Lye and chromium ion solution is added dropwise simultaneously, the degree of supersaturation of chromium hydroxide nucleation can be reduced, increase it with heterogeneous nucleation side
The probability of formula forming core makes chromium preferably be distributed in the surface of magnesia.
In addition, the technology of the present invention exploitation early stage, attempts by way of ball milling, by Cr2O3It mixes in magnesia, is formed and contain chromium
Magnesia, finally calcining obtains mixing the magnesia spinel phase of chromium at 1600 DEG C, and tests its mechanism of its performance study, but due to passing through
Physical doping but that can use method used in the present invention instead and study due to polluted product and higher cost etc..Pass through this
The heavy chromium reaction of invention, cooperates subsequent tabletting and calcining mechanism, can make chrome green original position, Uniform Doped to magnesia
In, the uniformity of obtained material is more preferable.
Claims (7)
1. a kind of preparation method containing chrome-magnesite, which is characterized in that by lye and contain Cr3+Solion, which synchronizes, to be added dropwise to containing oxidation
In the aqueous solution in magnesium source, in 30~75 DEG C of the heavy chromium reaction of at a temperature of progress magnesium oxide source grain surface；After the reaction was completed through solid
Liquid separation, obtains presoma containing chrome-magnesite；The presoma containing chrome-magnesite first carries out one-step calcination at 900 ± 50 DEG C；One
The product of step calcining carries out two step calcinings at 1600 ± 50 DEG C again after compressing tablet process, obtains containing chrome-magnesite；
The solution containing magnesium oxide source is the aqueous solution for being dispersed with magnesium oxide source；In the solution containing magnesium oxide source, admittedly contain
Amount is 20~45wt%；
Again through the compressing tablet process after the one-step calcination product and adhesive mixing；
The adhesive is PVA, sodium carboxymethylcellulose, one kind in chitosan at least within；The adhesive adds
Dosage is 1~3wt% of one-step calcination products weight.
2. as described in claim 1 containing the preparation method of chrome-magnesite, which is characterized in that the lye is alkali metal hydroxide
The mixed liquor of the aqueous solution of object, ammonium hydroxide or said two devices；
The pH of the lye is 9~13.
3. as described in claim 1 containing the preparation method of chrome-magnesite, which is characterized in that contain Cr3+Solion is chromic salt
Aqueous solution；Wherein, Cr3+Concentration be 0.2~0.4mol/L.
4. as described in claim 1 containing the preparation method of chrome-magnesite, which is characterized in that the solution containing magnesium oxide source is point
Dissipate the aqueous solution for having magnesium oxide source；In the solution containing magnesium oxide source, solid content is 35~45wt%.
5. as described in claim 1 containing the preparation method of chrome-magnesite, which is characterized in that the temperature of heavy chromium reaction process is 40~
60℃。
6. as claimed in claim 5 containing the preparation method of chrome-magnesite, which is characterized in that the time of heavy chromium reaction is 0.5~2h；
The mixing speed of heavy chromium reaction process is 200~650r/min.
7. as described in claim 1 containing the preparation method of chrome-magnesite, which is characterized in that the time of one-step calcination is 1~2h；Two
The time of step calcining is 3~4h.
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| CN114368973A (en) * | 2021-12-24 | 2022-04-19 | 江苏材睿科技有限公司 | Formula, production process and method of environment-friendly refractory material |
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|---|---|---|---|---|
| DD232904A1 (en) * | 1984-12-27 | 1986-02-12 | Kali Veb K | METHOD FOR PRODUCING HIGH-PURITY SINTERMAGNESIA HIGH DENSITY |
| CN1172768A (en) * | 1997-08-29 | 1998-02-11 | 高耀军 | Method for producing electric smelting high-purity magnesite suitable for plateau environment |
| CN102295462A (en) * | 2011-05-31 | 2011-12-28 | 浙江大学 | Magnesium-chromium hollow ball and preparation method thereof |
| CN108046620A (en) * | 2017-12-08 | 2018-05-18 | 中南大学 | It is a kind of that the method containing chrome-magnesite is prepared by magnesite light burnt powder |
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2017
- 2017-10-13 CN CN201710956812.7A patent/CN107585779B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD232904A1 (en) * | 1984-12-27 | 1986-02-12 | Kali Veb K | METHOD FOR PRODUCING HIGH-PURITY SINTERMAGNESIA HIGH DENSITY |
| CN1172768A (en) * | 1997-08-29 | 1998-02-11 | 高耀军 | Method for producing electric smelting high-purity magnesite suitable for plateau environment |
| CN102295462A (en) * | 2011-05-31 | 2011-12-28 | 浙江大学 | Magnesium-chromium hollow ball and preparation method thereof |
| CN108046620A (en) * | 2017-12-08 | 2018-05-18 | 中南大学 | It is a kind of that the method containing chrome-magnesite is prepared by magnesite light burnt powder |
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