CN103539162B - Process method for preparing ammonium-potassium sulfate from potassium feldspar - Google Patents
Process method for preparing ammonium-potassium sulfate from potassium feldspar Download PDFInfo
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- CN103539162B CN103539162B CN201310526092.2A CN201310526092A CN103539162B CN 103539162 B CN103539162 B CN 103539162B CN 201310526092 A CN201310526092 A CN 201310526092A CN 103539162 B CN103539162 B CN 103539162B
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Abstract
The invention relates to a method for preparing ammonium-potassium sulfate from potassium feldspar. The process method for preparing the ammonium-potassium sulfate from the potassium feldspar comprises the following steps: 1) decomposing potassium feldspar; 2) leaching a reaction solid, namely, leaching the solid residue obtained after the reaction of potassium feldspar through an acid solution with volume fraction of 8 to 10% at 90 to 110 DEG C, and filtering the leached serous fluid through a filter; 3) preparing calcium sulfate whiskers, namely, adding a seed crystal to filtrate, agitating and dissolving, and ageing at room temperature to prepare the calcium sulfate whiskers; 4) preparing aluminum hydroxide and iron oxide red, namely, neutralizing the filtrate obtained after the calcium sulfate whiskers are prepared through ammonia water in order to precipitate ferric ion, and then adding ammonia water or potassium hydroxide to the filtrate to precipitate aluminum ions; and 5) preparing ammonium-potassium sulfate, namely, concentrating the filtrate in a vacuum way until saturating, wherein the concentration temperature is controlled to be 45 to 55 DEG C, and the vacuum degree is controlled to be 0.08 to 0.12MPa, enabling an ammonium-potassium sulfate crystal to be separated out, and then carrying out spraying granulation and drying to obtain a binary compound fertilizer, namely, ammonium-potassium sulfate.
Description
Technical field
The present invention relates to a kind of method utilizing potassium felspar sand extracting sulfuric acid ammonium potassium, be specifically related to a kind of method from potassium feldspar decomposition residue leaching liquid extracting sulfuric acid ammonium K composite fertilizer.
Background technology
The identified soluble potassium salt resource reserve of China is little, is difficult to meet the demand of agricultural to potash fertilizer.Up to the present, the potash fertilizer of China 70% needs import.Exactly because the reserves of China's soluble potassium salt resource are less, therefore, sylvite ore is listed in one of Critical needed mineral species by country.But the insoluble Potash Resources of China but rich reserves, be that the insoluble of representative almost spreads all over China's major part provinces and regions containing sylvite rock, the about tens billion of ton of its geology reserves with potassium felspar sand.If therefore can by furtheing investigate further potassium feldspar decomposition comprehensive utilization technique, find out that a set of comprehensive utilization degree is high, technique is advanced, economically viable technology, will Great significance be had.
Summary of the invention
The present invention is directed to the problem that background technology proposes, propose a kind of processing method of extracting sulfuric acid ammonium potassium from potassium felspar sand.Effectively make use of the potassium contained in potassium felspar sand, extracting sulfuric acid ammonium K composite fertilizer, for agriculture production.
To achieve these goals, the technical solution adopted in the present invention is:
(1) potassium feldspar decomposition reaction: after potassium felspar sand, fluorite, Neutral ammonium fluoride, the vitriol oil fully being mixed, join in converter reactor, reacts under 180 ~ 250 DEG C and autogenous pressure; Gas reaction produced introduces dedusting in dust removal filter, for subsequent production technique;
(2) react the leaching of solid: reacted for potassium felspar sand Reaktionsofen solid residue is proceeded to leaching groove by discharging spiral, at 90 ~ 110 DEG C, be the acid solution leaching of 8 ~ 10% by volume fraction, the slurries after leaching are filtered by filter;
(3) preparation of calcium sulfate crystal whiskers: the filtrate filtered out is got in crystal of calcium sulfate still by pump, and in filtrate, add crystal seed (magnesium salts) stirring and dissolving, slowly be down to room temperature and carry out ageing, generate calcium sulfate crystal whiskers, through Filter Press, dry obtained calcium sulfate crystal whiskers;
(4) preparation of aluminium hydroxide and iron oxide red: the filtrate after extracting sulfuric acid calcium pyroborate first with ammonia neutralization to pH ≈ 3.5 ~ 5 precipitation of iron ions out, filtration drying roasting obtains iron oxide red;
Filtrate adds ammoniacal liquor again and adjusts pH ≈ 7.5 ~ 8.5, or hydro-oxidation potassium adjusts pH ≈ about 8 ~ 10, then aluminum ion is precipitated out, and filtration drying obtains aluminium hydroxide;
(5) preparation of ammonium-potassium sulfate: above-mentioned filtrate is by vacuum concentration to saturated, and thickening temperature controls at 45 ~ 55 DEG C, and vacuum degree control, at 0.08 ~ 0.12MPa, makes ammonium-potassium sulfate crystal separate out; Then spray granulating, be drying to obtain binary compound fertilizer ammonium-potassium sulfate.
The processing method of described extracting sulfuric acid ammonium potassium from potassium felspar sand, in potassium feldspar decomposition reaction process, potassium felspar sand, fluorite, Neutral ammonium fluoride, sulfuric acid mass ratio are 1:0.3 ~ 0.5:1.12 ~ 1.73:1.6 ~ 1.8, wherein sulfuric acid consumption by 98% the vitriol oil, the reaction times controlled at 2 ~ 4.5 hours.
The processing method of described extracting sulfuric acid ammonium potassium from potassium felspar sand, in the preparation process of calcium sulfate crystal whiskers, the filtrate filtered out is got in crystal of calcium sulfate still by pump, and in filtrate, add crystal seed (magnesium salts) stirring and dissolving, slowly be down to room temperature and carry out ageing, crystallization, crystallization time controls at 7.5 ~ 8.5 hours; The amount adding crystal seed in filtrate is 2 ~ 3% of potassium feldspar decomposition mass of residue, and stirring velocity is 30 ~ 80 r/min.
The processing method of described extracting sulfuric acid ammonium potassium from potassium felspar sand, in the preparation process of aluminium hydroxide and iron oxide red, the filtrate after extracting sulfuric acid calcium pyroborate first with ammonia neutralization to pH ≈ 4 precipitation of iron ions out, filtration drying roasting obtains iron oxide red; Adding ammoniacal liquor again adjusts pH ≈ 8 that aluminum ion is precipitated out, and filtration drying obtains aluminium hydroxide;
The processing method of described extracting sulfuric acid ammonium potassium from potassium felspar sand, in the leaching process of reaction solid, leaching temperature controls at 100 DEG C, adopt volume fraction be 10% sulphuric acid soln leaching; In the preparation process of ammonium-potassium sulfate, thickening temperature controls at 50 DEG C, and vacuum degree control is at 0.1MPa.
The useful positively effect of invention:
1, the processing method of the present invention's extracting sulfuric acid ammonium potassium from potassium felspar sand, makes the effective constituent of potassium felspar sand be fully used, improves the comprehensive utilization technique of potassium felspar sand.Described processing method, after potassium felspar sand, fluorite and sulfuric acid fully being mixed, joins in converter reactor, react at 180 ~ 250 DEG C, the SiF that reaction produces
4separate from system under condition of negative pressure with HF gas, and carry out absorption by ethanol and the aqueous solution and prepare white carbon black, reacted solid, by series of process such as leachings, obtains mainly containing K
+and Al
3+leaching liquid, for the preparation of aluminium hydroxide and ammonium-potassium sulfate product.
2, the processing method of the present invention's extracting sulfuric acid ammonium potassium from potassium felspar sand, adopt the technique of low temperature semidrying decomposing of potassium feldspar, temperature of reaction is at 180 ~ 250 DEG C, compared with pyroprocess decomposing of potassium feldspar, reaction conditions is gentle, and lower to the requirement of equipment, subsequent treatment process is simple and easy to do.
3, the processing method of the present invention's extracting sulfuric acid ammonium potassium from potassium felspar sand, can make Si, K, Fe, Al composition in potassium felspar sand all be fully utilized, for the preparation of white carbon black, aluminium hydroxide, iron oxide red and ammonium-potassium sulfate composite fertilizer.Contribute to economizing on resources, reduce waste and environment protection.It is promoted the use of, and will produce good society and economic implications.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
embodiment 1
The processing method of the present invention's extracting sulfuric acid ammonium potassium from potassium felspar sand, step is as follows:
(1) potassium feldspar decomposition reaction:
By potassium felspar sand, fluorite, Neutral ammonium fluoride, 98% sulfuric acid fully mix after, join in converter reactor, react under 180 ~ 250 DEG C and autogenous pressure; Reaction principle is:
CaF
2?+?H
2SO
4?=?2HF?+?CaSO
4
2K[AlSi
3O
8]?+?24HF?+?4H
2SO
4?=?K
2SO
4?+?Al
2(SO
4)
3?+?6SiF
4↑+?16H
2O
Wherein, potassium felspar sand, fluorite, Neutral ammonium fluoride, 98% sulfuric acid mass ratio be 1:0.3 ~ 0.5:1.12 ~ 1.73:1.6 ~ 1.8.The gas produced removes absorption system, and potassium feldspar decomposition residue goes leaching.
(2) leaching of solid is reacted:
Reacted for potassium felspar sand Reaktionsofen solid residue is proceeded to leaching groove by discharging spiral, at 100 DEG C, be the acid solution leaching of 10% by volume fraction, solid-to-liquid ratio is 1:5 ~ 10, the filtrate that filtered while hot goes out is for subsequent production technique, and residue is for the production of aerated bricks.
(3) preparation of calcium sulfate crystal whiskers: the filtrate filtered out is got in crystal of calcium sulfate still by pump, and in filtrate, add crystal seed (magnesium salts) stirring and dissolving, the amount adding crystal seed is 2 ~ 3% of potassium feldspar decomposition mass of residue, slowly be down to room temperature and carry out ageing, the calcium sulfate crystal whiskers of generation is through Filter Press, dry obtained calcium sulfate crystal whiskers.
(4) preparation of aluminium hydroxide and iron oxide red: the filtrate after extracting sulfuric acid calcium pyroborate first with ammonia neutralization to pH ≈ 4 precipitation of iron ions out, filtration drying roasting obtains iron oxide red; Adding ammoniacal liquor again adjusts pH ≈ 8 that aluminum ion is precipitated out, filtration, dry obtained aluminium hydroxide.
(5) preparation of ammonium-potassium sulfate: above-mentioned filtrate is by vacuum concentration to saturated, and ammonium-potassium sulfate crystal is separated out; Concentrated condition: temperature is at about 50 DEG C, and vacuum tightness is about 0.1MPa.Then spray granulating, be drying to obtain binary compound fertilizer.
embodiment 2
The processing method of the present embodiment extracting sulfuric acid ammonium potassium from potassium felspar sand, be with the difference of embodiment 1: in the preparation process of calcium sulfate crystal whiskers, the filtrate filtered out is got in crystal of calcium sulfate still by pump, and in filtrate, add crystal seed (magnesium salts) stirring and dissolving, slowly be down to room temperature and carry out ageing, crystallization, crystallization time controls at 7.5 ~ 8.5 hours; The amount adding crystal seed in filtrate is 2 ~ 3% of potassium feldspar decomposition mass of residue, and stirring velocity is 30 ~ 80 r/min.
embodiment 3
The processing method of the present embodiment extracting sulfuric acid ammonium potassium from potassium felspar sand, be with the difference of embodiment 1 or embodiment 2: in the preparation process of step (4) aluminium hydroxide and iron oxide red, filtrate after extracting sulfuric acid calcium pyroborate first with ammonia neutralization to pH ≈ about 4 ~ 5, precipitation of iron ions out, filtration drying roasting obtains iron oxide red; Filtrate repeated hydrogenation potassium oxide adjusts pH ≈ about 8 ~ 10, and aluminum ion is precipitated out, and filtration drying obtains aluminium hydroxide; Filtrate evaporation concentration obtains ammonium-potassium sulfate crystal, then spray granulating, be drying to obtain binary compound fertilizer.
Claims (5)
1. the processing method of extracting sulfuric acid ammonium potassium from potassium felspar sand, comprises the steps:
(1) potassium feldspar decomposition reaction: after potassium felspar sand, fluorite, Neutral ammonium fluoride, the vitriol oil fully being mixed, join in converter reactor, reacts under 180 ~ 250 DEG C and autogenous pressure; Gas reaction produced introduces dedusting in dust removal filter, prepares white carbon black for sequential hydrolysis;
(2) react the leaching of solid: reacted for potassium felspar sand Reaktionsofen solid residue is proceeded to leaching groove by discharging spiral, at 90 ~ 110 DEG C, be the acid solution leaching of 8 ~ 10% by volume fraction, the slurries after leaching are filtered by filter;
(3) preparation of calcium sulfate crystal whiskers: the filtrate filtered out is got in crystal of calcium sulfate still by pump, and crystal seed stirring and dissolving is added in filtrate, be slowly down to room temperature and carry out ageing, generate calcium sulfate crystal whiskers, through Filter Press, dry obtained calcium sulfate crystal whiskers;
(4) preparation of aluminium hydroxide and iron oxide red: the filtrate after extracting sulfuric acid calcium pyroborate first with ammonia neutralization to pH ≈ 3.5 ~ 5 precipitation of iron ions out, filtration drying roasting obtains iron oxide red; Filtrate adds ammoniacal liquor again and adjusts pH ≈ 7.5 ~ 8.5, or hydro-oxidation potassium adjusts pH ≈ about 8 ~ 10, then aluminum ion is precipitated out, and filtration drying obtains aluminium hydroxide;
(5) preparation of ammonium-potassium sulfate: above-mentioned filtrate is by vacuum concentration to saturated, and thickening temperature controls at 45 ~ 55 DEG C, and vacuum degree control, at 0.08 ~ 0.12MPa, makes ammonium-potassium sulfate crystal separate out; Then spray granulating, be drying to obtain binary compound fertilizer ammonium-potassium sulfate.
2. the processing method of extracting sulfuric acid ammonium potassium from potassium felspar sand according to claim 1, it is characterized in that: in potassium feldspar decomposition reaction process, potassium felspar sand, fluorite, Neutral ammonium fluoride, sulfuric acid mass ratio are 1:0.3 ~ 0.5:1.12 ~ 1.73:1.6 ~ 1.8, wherein sulfuric acid consumption by 98% the vitriol oil, the reaction times controlled at 2 ~ 4.5 hours.
3. the processing method of extracting sulfuric acid ammonium potassium from potassium felspar sand according to claim 1, it is characterized in that: in the preparation process of calcium sulfate crystal whiskers, the filtrate filtered out is got in crystal of calcium sulfate still by pump, and crystal seed stirring and dissolving is added in filtrate, slowly be down to room temperature and carry out ageing, crystallization, crystallization time controls at 7.5 ~ 8.5 hours; The amount adding crystal seed in filtrate is 2 ~ 3% of potassium feldspar decomposition mass of residue, and stirring velocity is 30 ~ 80 r/min.
4. the processing method of extracting sulfuric acid ammonium potassium from potassium felspar sand according to claim 1,2 or 3, it is characterized in that: in the preparation process of aluminium hydroxide and iron oxide red, filtrate after extracting sulfuric acid calcium pyroborate first with ammonia neutralization to pH ≈ 4 precipitation of iron ions out, filtration drying roasting obtains iron oxide red; Adding ammoniacal liquor again adjusts pH ≈ 8 that aluminum ion is precipitated out, and filtration drying obtains aluminium hydroxide.
5. the processing method of extracting sulfuric acid ammonium potassium from potassium felspar sand according to claim 4, is characterized in that: in the leaching process of reaction solid, leaching temperature controls at 100 DEG C, and employing volume fraction is the sulphuric acid soln leaching of 10%; In the preparation process of ammonium-potassium sulfate, thickening temperature controls at 50 DEG C, and vacuum degree control is at 0.1MPa.
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Owner name: LUOYANG FLUORIDE + POTASSIUM TECHNOLOGY COMPANY Free format text: FORMER NAME: LUOYANG FLUORIDE + POTASSIUM TECHNOLOGY LTD. |
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Address after: 471400, Henan, Luoyang province Songxian meal slope Township Industrial Agglomeration Patentee after: LUOYANG FLUORIDE & POTASSIUM TECHNOLOGY CO., LTD. Address before: 471400, Luoyang, Songxian, Henan province Township Po Industrial Agglomeration Area Luoyang fluorine potassium Technology Co., Ltd. Patentee before: Luoyang Fluofide & Potassium Technology Co., Ltd. |