CN105060350A - Production method of iron oxide by utilizing potassium-bearing rock - Google Patents
Production method of iron oxide by utilizing potassium-bearing rock Download PDFInfo
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- CN105060350A CN105060350A CN201510470899.8A CN201510470899A CN105060350A CN 105060350 A CN105060350 A CN 105060350A CN 201510470899 A CN201510470899 A CN 201510470899A CN 105060350 A CN105060350 A CN 105060350A
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Abstract
The present invention discloses a production method of iron oxide by utilizing potassium-bearing rock, and belongs to the technical field of chemical engineering. The method is as below: first pulverizing potassium rock, then mixing and reacting the rock powder with fluorosilicic acid and sulfuric acid in a microwave reaction vessel, separating the reaction products, subjecting the separated solids with water and ammonia to a neutralization reaction, then conducting solid-liquid separation, mixing the separated solid with sodium hydroxide, carrying out microwave treatment, and calcining the solids obtain from the solid-liquid separation into a microwave reactor at high temperature, so as to obtain the iron oxide product. Compare with the precipitation process for iron removal in the traditional utilization of potassium bearing rock, the method makes full use of element iron to prepare iron oxide, further increases the added value of potassium-bearing rock, fully uses the element iron in the potassium-bearing rock, and simplifies the synthetic process of iron red.
Description
Technical field
The present invention relates to chemical production technical field, specifically, relate to a kind of method utilizing potassium bearing rock to prepare ferric oxide.
Background technology
China's potassium bearing rock reserves are abundanter, the explored potassium bearing rock resource of China reaches 30,000,000,000 tons according to statistics, the low-temperature decomposition potassium bearing rock method of comprehensive utilization that studies in China is more, as patent CN200410023558.8 discloses a kind of low temperature decomposition method for potassium feldspar, its mixing acid adopting silicofluoric acid to add sulfuric acid carrys out decomposing of potassium feldspar, utilize the high boiling point of sulfuric acid that silicofluoric acid is all converted into silicon tetrafluoride, and then enter absorption tower recovery silicofluoric acid, the general evaporation time of the method is more than 8 hours, need a large amount of energy consumption, approximately often process one ton of potassium felspar sand to need to consume 1.0 tons, the coal that heat content is 5000 kilocalories, increase production cost, and treatment process is loaded down with trivial details, benefit is lower.Patent CN201010280115.2 discloses a kind of method processing potassium bearing rock, that potassium bearing rock is crushed to 100 ~ 200 orders, then auxiliary agent silicofluoric acid is utilized to decompose potassium bearing rock, react after 1 ~ 3 hour, obtain the mixture comprising potassium silicofluoride, aluminum fluosilicate and silica gel, silicofluoric acid is reclaimed in acidifying again, obtains potash fertilizer products.Although the method has saved the energy consumption of 60 ~ 80% than nitration mixture steam seasoning, shorten the time of 4 ~ 6 times, the time is still long, and the molten potassium promoter rate of recovery is not high.Above-mentioned cryogenic treatment process, General reactions was for up to 2 ~ 3 hours, and need 5 ~ 8 filtering separation, 3 ~ 6 dryings, complex process, energy consumption is huge, and product purity is low, was separated not thorough, low in economic efficiency.
Method red iron oxide being prepared by iron-bearing material is a lot, common are dry method and wet method.Green vitriol calcination method SO in dry method
2and SO
3generation very easily cause environmental pollution and equipment corrosion; Sulphate process in wet processing, nitrate process and nitration mixture salt method all need to manufacture crystal seed, and shortcoming is technique comparatively complexity, long reaction time, uneconomical etc.; The more hydro-thermal rule of recent research needs the requirement of autoclave to equipment higher.
Summary of the invention
In view of this, the object of this invention is to provide a kind of method utilizing potassium bearing rock to prepare ferric oxide, the method adopts three microwave technologies to decompose potassium bearing rock and produces ferric oxide, and the ferro element in comprehensive utilization potassium bearing rock improves added value, has the advantages such as technique is simple, additive is few.
For achieving the above object, the present invention adopts following technical scheme:
Utilize potassium bearing rock to prepare a method for ferric oxide, comprise the following steps:
(1) microwave reaction: first potassium bearing rock is pulverized, then by potassium bearing rock powder with silicofluoric acid, sulfuric acid according to 1:(1 ~ 2): the volume ratio of (0.1 ~ 0.55) mixes, be placed in microwave reaction kettle, adjustment microwave power is 1 ~ 27.5kw, obtains solid I after reaction 1 ~ 5.5h;
(2) neutralization reaction: mixed according to a certain percentage with water, ammoniacal liquor by solid I and carry out neutralization reaction, carries out solid-liquid separation after reaction for some time, obtains solid II and liquid I;
(3) secondary microwave reaction: send in microwave reaction kettle after being mixed with sodium hydroxide by solid II and carry out microwave treatment, control temperature is 80 ~ 150 DEG C, after reaction for some time, carries out solid-liquid separation and obtains solid III;
(4) three microwave reactions: send in microwave reactor by solid III, adopt the high-temperature calcination 1 ~ 4h of 300 ~ 800 DEG C, obtain iron oxide product.
The concentration of described silicofluoric acid is 20 ~ 40%.
The concentration of described sulfuric acid is 30 ~ 98%.
In described step (1), first potassium bearing rock being ground into fineness is 100 ~ 300 object fine powders, then be 25 ~ 35% silicofluoric acid by potassium bearing rock powder and concentration, concentration is that 40 ~ 80% sulfuric acid mix according to the volume ratio of 1:1.5:0.3, be placed in microwave reaction kettle, adjustment microwave power is 10 ~ 20kw, obtains solid I after reaction 3 ~ 5h.
In described step (2), by solid I with water, ammoniacal liquor according to 1:(1 ~ 3): the volume ratio of (0.7 ~ 2) mixes carries out neutralization reaction, reaction 20 ~ 60min after carry out solid-liquid separation, obtain solid II and liquid I.
The concentration of described ammoniacal liquor is 10 ~ 32%.
In described step (3), by solid II with sodium hydroxide with 1:(2 ~ 8) volume ratio mix after send in microwave reaction kettle and carry out microwave treatment, control microwave power is 6 ~ 25kw, temperature of reaction is 80 ~ 150 DEG C, after reaction 1 ~ 3h, carry out solid-liquid separation and obtain solid III.
The concentration of described sodium hydroxide is 10 ~ 40%.
In described step (4), send in microwave reactor by solid III, control microwave power is 10 ~ 70kw, adopts the high-temperature calcination 1 ~ 4h of 300 ~ 800 DEG C, obtains iron oxide product.
Beneficial effect of the present invention is: the present invention utilizes the distinctive character of microwave, directly acts on material molecule, makes phase mutual friction between molecule, produces amount of heat, and then impels reaction to carry out, substantially reduce the reaction times, be only 1/6 of the traditional method reaction times; In potassium bearing rock potassium, the extraction rate reached of potassium is to more than 99%.The present invention adopts three microwave technologies decomposition potassium bearing rocks to prepare ferric oxide, enormously simplify the production technique of ferric oxide, valuable element in potassium bearing rock is utilized, to utilize in technique compared with precipitator method deironing with traditional potassium bearing rock, make full use of ferro element and prepare ferric oxide, the added value of further raising potassium bearing rock, had both taken full advantage of the ferro element in potassium bearing rock, in turn simplify the synthesis technique of red iron oxide.
Embodiment
Conveniently those skilled in the art will recognize that the present invention will be further described below in conjunction with embodiment.Embodiment is only illustrating this invention, is not limitation of the invention, and the step not doing in embodiment to illustrate is all prior arts, is not described in detail at this.
Embodiment one
A kind of method utilizing potassium bearing rock to prepare ferric oxide, first potassium bearing rock being ground into fineness is 100 object fine powders, then be 20% silicofluoric acid by potassium bearing rock powder and concentration, concentration is that 30 ~ 98% sulfuric acid mix according to the volume ratio of 1:1:0.1, be placed in microwave reaction kettle, adjustment microwave power is 1kw, obtains solid I after reaction 1h; Be that 10% ammoniacal liquor mixes according to the volume ratio of 1:1:0.7 and carries out neutralization reaction by solid I and water, concentration, carry out solid-liquid separation after reaction 20min, obtain solid II and liquid I; Be send in microwave reaction kettle after 10% sodium hydroxide mixes with the volume ratio of 1:2 to carry out microwave treatment by solid II and concentration, control microwave power is 6kw, and temperature of reaction is 80 DEG C, after reaction 1h, carries out solid-liquid separation and obtains solid III; Send in microwave reactor by solid III, control microwave power is 10kw, adopts the high-temperature calcination 1h of 300 DEG C, obtains iron oxide product.
Embodiment two
A kind of method utilizing potassium bearing rock to prepare ferric oxide, first potassium bearing rock being ground into fineness is 300 object fine powders, then be 40% silicofluoric acid by potassium bearing rock powder and concentration, concentration is that 98% sulfuric acid mixes according to the volume ratio of 1:2:0.55, be placed in microwave reaction kettle, adjustment microwave power is 27.5kw, obtains solid I after reaction 5.5h; Be that 32% ammoniacal liquor mixes according to the volume ratio of 1:3:2 and carries out neutralization reaction by solid I and water, concentration, carry out solid-liquid separation after reaction 60min, obtain solid II and liquid I; Be send in microwave reaction kettle after 40% sodium hydroxide mixes with the volume ratio of 1:8 to carry out microwave treatment by solid II and concentration, control microwave power is 25kw, and temperature of reaction is 150 DEG C, after reaction 3h, carries out solid-liquid separation and obtains solid III; Send in microwave reactor by solid III, control microwave power is 70kw, adopts the high-temperature calcination 4h of 800 DEG C, obtains iron oxide product.
Embodiment three
A kind of method utilizing potassium bearing rock to prepare ferric oxide, first potassium bearing rock being ground into fineness is 160 object fine powders, then be 25% silicofluoric acid by potassium bearing rock powder and concentration, concentration is that 40% sulfuric acid mixes according to the volume ratio of 1:2:0.2, be placed in microwave reaction kettle, adjustment microwave power is 10kw, obtains solid I after reaction 2h; Be that 16% ammoniacal liquor mixes according to the volume ratio of 1:2:1 and carries out neutralization reaction by solid I and water, concentration, carry out solid-liquid separation after reaction 30min, obtain solid II and liquid I; Be send in microwave reaction kettle after 20% sodium hydroxide mixes with the volume ratio of 1:3 to carry out microwave treatment by solid II and concentration, control microwave power is 10kw, and temperature of reaction is 90 DEG C, after reaction 2h, carries out solid-liquid separation and obtains solid III; Send in microwave reactor by solid III, control microwave power is 20kw, adopts the high-temperature calcination 2h of 400 DEG C, obtains iron oxide product.
Embodiment four
A kind of method utilizing potassium bearing rock to prepare ferric oxide, first potassium bearing rock being ground into fineness is 200 object fine powders, then be 35% silicofluoric acid by potassium bearing rock powder and concentration, concentration is that 80% sulfuric acid mixes according to the volume ratio of 1:2:0.4, be placed in microwave reaction kettle, adjustment microwave power is 20kw, obtains solid I after reaction 3h; Be that 25% ammoniacal liquor mixes according to the volume ratio of 1:2:1.5 and carries out neutralization reaction by solid I and water, concentration, carry out solid-liquid separation after reaction 50min, obtain solid II and liquid I; Be send in microwave reaction kettle after 30% sodium hydroxide mixes with the volume ratio of 1:7 to carry out microwave treatment by solid II and concentration, control microwave power is 20kw, and temperature of reaction is 120 DEG C, after reaction 2.5h, carries out solid-liquid separation and obtains solid III; Send in microwave reactor by solid III, control microwave power is 60kw, adopts the high-temperature calcination 3h of 600 DEG C, obtains iron oxide product.
Embodiment five
A kind of method utilizing potassium bearing rock to prepare ferric oxide, first potassium bearing rock being ground into fineness is 120 object fine powders, then be 30% silicofluoric acid by potassium bearing rock powder and concentration, concentration is that 60% sulfuric acid mixes according to the volume ratio of 1:1.5:0.3, be placed in microwave reaction kettle, adjustment microwave power is 14kw, obtains solid I after reaction 3h; Be that 16% ammoniacal liquor mixes according to the volume ratio of 1:2:1.5 and carries out neutralization reaction by solid I and water, concentration, carry out solid-liquid separation after reaction 40min, obtain solid II and liquid I; Be send in microwave reaction kettle after 25% sodium hydroxide mixes with the volume ratio of 1:5 to carry out microwave treatment by solid II and concentration, control microwave power is 14kw, and temperature of reaction is 100 DEG C, after reaction 2h, carries out solid-liquid separation and obtains solid III; Send in microwave reactor by solid III, control microwave power is 40kw, adopts the high-temperature calcination 3h of 500 DEG C, obtains iron oxide product.
The above, it is only better example of the present invention, not any pro forma restriction is done to the present invention, anyly do not depart from technical solution of the present invention content, the any simple modification done above example according to technical spirit of the present invention, coversion material equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (9)
1. utilize potassium bearing rock to prepare a method for ferric oxide, it is characterized in that, comprise the following steps:
(1) microwave reaction: first potassium bearing rock is pulverized, then by potassium bearing rock powder with silicofluoric acid, sulfuric acid according to 1:(1 ~ 2): the volume ratio of (0.1 ~ 0.55) mixes, be placed in microwave reaction kettle, adjustment microwave power is 1 ~ 27.5kw, obtains solid I after reaction 1 ~ 5.5h;
(2) neutralization reaction: mixed according to a certain percentage with water, ammoniacal liquor by solid I and carry out neutralization reaction, carries out solid-liquid separation after reaction for some time, obtains solid II and liquid I;
(3) secondary microwave reaction: send in microwave reaction kettle after being mixed with sodium hydroxide by solid II and carry out microwave treatment, control temperature is 80 ~ 150 DEG C, after reaction for some time, carries out solid-liquid separation and obtains solid III;
(4) three microwave reactions: send in microwave reactor by solid III, adopt the high-temperature calcination 1 ~ 4h of 300 ~ 800 DEG C, obtain iron oxide product.
2. utilize potassium bearing rock to prepare the method for ferric oxide as claimed in claim 1, it is characterized in that, the concentration of described silicofluoric acid is 20 ~ 40%.
3. utilize potassium bearing rock to prepare the method for ferric oxide as claimed in claim 1, it is characterized in that, the concentration of described sulfuric acid is 30 ~ 98%.
4. utilize potassium bearing rock to prepare the method for ferric oxide as claimed in claim 1, it is characterized in that, in described step (1), first potassium bearing rock being ground into fineness is 100 ~ 300 object fine powders, then be 25 ~ 35% silicofluoric acid by potassium bearing rock powder and concentration, concentration is that 40 ~ 80% sulfuric acid mix according to the volume ratio of 1:1.5:0.3, be placed in microwave reaction kettle, adjustment microwave power is 10 ~ 20kw, obtains solid I after reaction 3 ~ 5h.
5. utilize potassium bearing rock to prepare the method for ferric oxide as claimed in claim 1, it is characterized in that, in described step (2), by solid I with water, ammoniacal liquor according to 1:(1 ~ 3): the volume ratio of (0.7 ~ 2) mixes carries out neutralization reaction, carry out solid-liquid separation after reaction 20 ~ 60min, obtain solid II and liquid I.
6. the potassium bearing rock that utilizes as described in claim 1 or 5 prepares the method for ferric oxide, it is characterized in that, the concentration of described ammoniacal liquor is 10 ~ 32%.
7. utilize potassium bearing rock to prepare the method for ferric oxide as claimed in claim 1, it is characterized in that, in described step (3), by solid II with sodium hydroxide with 1:(2 ~ 8) volume ratio mix after send in microwave reaction kettle and carry out microwave treatment, control microwave power is 6 ~ 25kw, temperature of reaction is 80 ~ 150 DEG C, after reaction 1 ~ 3h, carries out solid-liquid separation and obtains solid III.
8. the potassium bearing rock that utilizes as described in claim 1 or 7 prepares the method for ferric oxide, it is characterized in that, the concentration of described sodium hydroxide is 10 ~ 40%.
9. utilize potassium bearing rock to prepare the method for ferric oxide as claimed in claim 1, it is characterized in that, in described step (4), solid III is sent in microwave reactor, control microwave power is 10 ~ 70kw, adopts the high-temperature calcination 1 ~ 4h of 300 ~ 800 DEG C, obtains iron oxide product.
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CN104495889A (en) * | 2014-11-26 | 2015-04-08 | 贵州远盛钾业科技有限公司 | Method for processing potassium-containing rock through industrial microwave |
CN104556175A (en) * | 2015-01-22 | 2015-04-29 | 武汉理工大学 | Method for preparing aluminum hydroxide from potash feldspar decomposition tailings |
CN104760976A (en) * | 2015-03-20 | 2015-07-08 | 贵州远盛钾业科技有限公司 | Comprehensive utilization method of potassium-containing shale by microwave treatment |
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US6140001A (en) * | 1999-05-04 | 2000-10-31 | Mitsui Mining & Smelting Co., Ltd. | Iron oxide microparticles and a process for producing them |
CN1762832A (en) * | 2005-09-12 | 2006-04-26 | 鄂州市长润农业生态技术有限公司 | Potash feldspar deferrization concentrating and iron-oxide red production method |
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Application publication date: 20151118 |