CN103420399A - Method for extracting soluble potassium from potassium feldspar by using acid process - Google Patents
Method for extracting soluble potassium from potassium feldspar by using acid process Download PDFInfo
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- CN103420399A CN103420399A CN2013103176646A CN201310317664A CN103420399A CN 103420399 A CN103420399 A CN 103420399A CN 2013103176646 A CN2013103176646 A CN 2013103176646A CN 201310317664 A CN201310317664 A CN 201310317664A CN 103420399 A CN103420399 A CN 103420399A
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Abstract
The invention discloses a method for extracting soluble potassium from potash feldspar by using an acid process. The method comprises the following steps: potash feldspar powder and low- concentration acid, assistant HF (hydrofluoric acid) or CaF2 (fluorite) are directly fed, and loaded into a closed liner monel 400 alloy or a liner tetrafluoro high pressure reactor for reaction, the product is cooled down to the room temperature, filtering is performed, underpressure distillation is performed on filter liquor, and solid, namely soluble sylvite, can be obtained after drying by distillation and cooling. In the method for extracting soluble potassium from potash feldspar by using the acid process, low-concentration acid, low-content HF or CaF2 is taken as an addition agent, under a low-temperature condition that the temperature does not exceed 150 DEG C, the internal structure of the potash feldspar can be effectively damaged, the extraction efficiency of the soluble potassium is increased, the productivity reaches more than 90 percent, the entire extracting process has the advantages of simple process, low temperature, less usage amount of acid and assistant, less environment pollution, high extraction efficiency, low cost and the like, and practical application and excellent industrialization prospect are achieved.
Description
Technical field
The invention belongs to field of inorganic chemical engineering, relate to a kind of method of extracting soluble potassium, relate in particular to a kind of method that acid system extracts soluble potassium in potassium felspar sand.
Background technology
The soluble potassium ionic compounds such as Repone K, salt of wormwood, vitriolate of tartar are the indispensable valuable cargos of industrial and agricultural production, and the national economic development is had to vital role.
At present, the present situation of China's potassium ore resources is: soluble potassium salt is extremely scarce, but the reserves of insoluble are abundanter, especially take potassium felspar sand as main refractory potassic mine stone reserves are large, it is wide to distribute, general potassium oxide content all is greater than 10%, therefore, carry out insoluble potassium Study on extraction, the refractory potassic mine resources such as existing potassium felspar sand of take are raw material, extract the soluble potassium of domestic production self-sufficiency, have important economy and strategic importance.
At present, extracting the comparatively typical technique of soluble potassium from potassium felspar sand has: (1) high-temperature calcination (as the kiln ash potash fertilizer method etc.), exist energy consumption high, the water consumption is high, and three waste discharge is serious; (2) microorganism decomposition method, this kind the method spawn culture cycle is long, the large-scale production technology is not mature enough.(3) hydrofluoric acid extraction method, this kind of scheme be because hydrofluoric acid corrodibility is large, to equipment require highly, and by product is too large, seriously polluted, the application limitation is larger; (4) ion exchange method, pollute littlely, and output is high, but the scale production difficulty is large, and cost is high.
The researcher of China utilizes acid system to extract soluble potassium from potassium felspar sand and obtains some progress, but still there is a significant limitation, main as follows: (1) Chinese patent ZL200710025493.4, with strong inorganic acid and the High hydrophilous resin of 1～7%WT, and the NaCl of 5～12 times of potassium felspar sand quality CaCl
2Na
2SO
4At 150～250 ℃, react K 1～4 hour
2O extraction yield>=70%, adopt this kind of technique extraction yield low, and the resin cost is high, without practical value; (2) Chinese patent ZL200410023558.8, utilize silicofluoric acid as auxiliary agent catalytic decomposition potassium felspar sand, take potassium felspar sand: 30% silicofluoric acid: 98% sulfuric acid is the proportioning of 1:3～10:0.025～3, and under 90 ℃～150 ℃ temperature condition, normal pressure decomposes 1 hour, K
2The O extraction yield can reach 99%, adopts this kind of technique need to consume the silicofluoric acid of a large amount of costlinesses, and high cost, be difficult to large-scale production, without practical value; (3) Chinese patent ZL200510019423.9, take potassium felspar sand: fluorite: 96～98 sulfuric acid are the proportioning of 1:1～2:2～3, under 50 ℃～80 ℃ temperature condition, normal pressure decomposes and prepares the potassium nitrogen composite fertilizer, and the soluble potassium extraction yield can reach 85～90%, adopt the extraction process of this patent, the fluorite consumption is bigger than normal, and waste residue is many, and normal pressure is easy to cause silicofluoric acid to overflow, cause environmental pollution, can't be applied to produce; (4) Chinese patent ZL200610019102.3, potassium felspar sand is with after the 30%HCl pickling, by potassium felspar sand: fluorite: water: and the proportioning that sulfuric acid is 1:2.4～2.5:1.8～2.2:3.5～3.6, at 85 ℃～95 ℃ temperature, reaction 1～3 h, normal pressure decomposes and prepares the potassium nitrogen composite fertilizer, and the potassium felspar sand extraction yield can reach 95%, adopts the technique of this patent, its technical problem and Chinese patent ZL200510019423.9 are similar, the fluorite consumption is bigger than normal, and waste residue is many, and environmental pollution is serious; (5) Chinese patent ZL200910015820.7, take potassium felspar sand: 30% silicofluoric acid: 98% sulfuric acid is the proportioning of 1:4.5:0. 5, at 100 ℃ of temperature, normal pressure decomposes 3 hours, potassium felspar sand extraction yield>=70%; Chinese patent ZL201010586310.8, take potassium felspar sand: the ratio that 15～30% silicofluoric acid+HF is 1:3, at 60～100 ℃ of temperature, normal pressure decomposes 4～6 hours, produces the potassium silicofluoride of 98% content, above two technical schemes that patent adopts, use a large amount of expensive silicofluoric acid, the hydrofluoric acid consumption is large simultaneously, high cost, and the practical application difficulty is large.
The applicant is engaged in the fundamental research of potassium felspar sand and the technical study of soluble powder sylvite for a long time, and structure and the physico-chemical property of potassium felspar sand had to comparatively deep understanding.The potassium felspar sand Main Components is the aluminum potassium silicate crystallization, and its chemical property is very stable, under normal temperature, is insoluble in the acid such as hydrochloric acid, sulfuric acid, only has hydrofluoric acid, and silicofluoric acid and highly basic can destroy the stable lattice of aluminum potassium silicate.The existing low temperature acid system of China extracts the method for soluble potassium in potassium felspar sand, is confined to the laboratory study stage more, and too high because of production cost, can't be applied to actual production.
Summary of the invention
The present invention is directed to existing soluble potassium extraction process, especially the technical problem of low temperature rapid extraction soluble potassium, provide that a kind of technique is simple, the auxiliary agent usage quantity is little, good product quality, extraction yield is high, good in economic efficiency, environmental pollution is little acid system extract the method for soluble potassium from potassium felspar sand.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method that acid system extracts soluble potassium from potassium felspar sand comprises the following steps:
(1) by potassium felspar sand powder, lower concentration mineral acid, auxiliary agent hydrofluoric acid (HF) or fluorite (CaF
2) directly feed intake, be loaded in airtight lining Monel 400 alloys or lining tetrafluoro autoclave and react;
(2) resultant of taking-up step (1) is cooled to room temperature, filters;
(3) filtrate in step (2) is carried out to underpressure distillation, evaporate to dryness, cooled solid are soluble potassium salt.
The present invention, on the basis of technique scheme, has done following improvement.
Preferably, the weight ratio of the potassium felspar sand powder in described step (1), lower concentration acid, auxiliary agent hydrofluoric acid or fluorite is 1:5～10:0.5～1.
Preferably, the lower concentration mineral acid preferably sulfuric acid (H in described step (1)
2SO
4) and hydrochloric acid (HCl), sulfuric acid (H
2SO
4) concentration is 2～5%, hydrochloric acid (HCl) concentration is 3～8%;
Preferably, the temperature of reaction in described step (1) in lining Monel 400 alloys or lining tetrafluoro autoclave is 90～150 ℃, and the reaction times is 5～12 hours.
The present invention is directed to the technical problem of existing low temperature rapid extraction soluble potassium, propose a kind of novel process of extracting soluble potassium based on acid system, its beneficial effect is:
1. acid system of the present invention extracts hydrofluoric acid (HF) or the fluorite (CaF that soluble potassium adopts lower concentration acid and low levels
2) as auxiliary agent, be no more than under the cold condition of 150 ℃, effectively destroyed the internal structure of potassium felspar sand, promoted the extraction yield of soluble potassium, productive rate reaches more than 90%;
2. the present invention relates to technique extract acid solution and auxiliary agent after soluble potassium salt can be by the underpressure distillation recovery, filter residue can be used as the white cement raw material, whole process is carried out under closed environment, the three wastes are accomplished zero release, save energy, and environmental contamination reduction;
Soluble potassium extraction process of the present invention possess that technique is simple, low temperature, low in the pollution of the environment, extraction yield advantages of higher, and lower concentration acid and hydrofluoric acid (HF) or fluorite (CaF
2) consumption few, greatly reduce production cost, practical application and industrial prospect are good.
The accompanying drawing explanation
Fig. 1 is that a kind of acid system of the present invention extracts the method for soluble potassium from potassium felspar sand.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing, the present invention is described in further detail, should be appreciated that concrete scheme described herein, only in order to explain the present invention, is not intended to limit the present invention.
As shown in Figure 1, by after potassium felspar sand raw ore Mechanical Crushing, obtain the potassium felspar sand powder, weight ratio by 1:5～10:0.5～1 directly feeds intake potassium felspar sand powder, lower concentration acid, hydrofluoric acid or fluorite, in airtight lining Monel 400 alloys that the temperature of packing into is 90～150 ℃ or lining tetrafluoro autoclave, reacts after 5～12 hours and takes out, and resultant is cooled to room temperature, filter, after filtrate is carried out rectification, after cooling 1～2h, can obtain soluble powder sylvite.
The method of with five embodiment, a kind of acid system of the present invention being extracted to soluble potassium from potassium felspar sand below is described in further detail.
Embodiment 1
Getting Xuyong County, Sichuan potassium oxide content is 1 kilogram of 11% potassium felspar sand, joins in the lining Monel 400 alloy autoclaves of 10L; The hydrochloric acid that adds 5 kilogram 5%; Add 500ml 30% hydrofluoric acid, closed reactor.Control 120 ℃ of temperature, reacting by heating 10 hours, finish reaction.Sampling, analyze the sour water reaction solution with the 6400A flame photometer, and potassium oxide content is 2.0%, finishes reaction.Be cooled to room temperature, filter, filtrate decompression distillation, capable of circulation the applying mechanically of hydrofluoric acid containing sour water distilled out.The solid obtained after evaporate to dryness is exactly 0.35 kilogram of the soluble potassium salt that extracts, with the 6400A flame photometer, analyzes, and potassium oxide content is 28.6%, and main component is Repone K and aluminum chloride, also has partial oxidation sodium.Through the present embodiment potassium extraction yield, be 91%.
Embodiment 2
Getting Wangcang County, Sichuan potassium oxide content is 1 kilogram of 13% potassium felspar sand, joins in the lining Monel 400 alloy autoclaves of 10L; The sulfuric acid that adds 5 kilogram 3%; Add 500ml 30% hydrofluoric acid, closed reactor.Control 150 ℃ of reacting by heating of temperature 8 hours, finish reaction.The potassium oxide content that sampling is analyzed the sour water reaction solution with the 6400A flame photometer is 2.4%, finishes reaction.Be cooled to room temperature, filter, filtrate decompression distillation, capable of circulation the applying mechanically of hydrofluoric acid containing sour water distilled out.The solid obtained after evaporate to dryness is exactly soluble potassium salt 520 grams that extract.With the 6400A flame photometer, analyze, potassium oxide content is 23.2%, and main component is sal enixum and Tai-Ace S 150, also has part of sulfuric acid hydrogen sodium.Through the present embodiment potassium extraction yield, be 93.1%.
Embodiment 3
Getting Xuyong County, Sichuan potassium oxide content is 10% potassium felspar sand double centner, joins in the lining tetrafluoro autoclave of 1000L; The hydrochloric acid that adds 800 kilogram 4%; Add 50 kilogram of 40% hydrofluoric acid, closed reactor.Control 110 ℃ of reacting by heating of temperature 12 hours, finish reaction.Sampling, the potassium oxide content of analyzing the sour water reaction solution with the 6400A flame photometer is 1.1%, finishes reaction.Be cooled to room temperature, filter, filtrate decompression distillation, capable of circulation the applying mechanically of hydrofluoric acid containing sour water distilled out.The solid obtained after evaporate to dryness is exactly 39 kilograms of the soluble potassium salts that extract.Main component is Repone K and aluminum chloride, a small amount of sodium-chlor.With the 6400A flame photometer, analyze, potassium oxide content is 23.8%, and the extraction yield of process the present embodiment potassium is 93%.
Embodiment 4
Getting Xuyong County, Sichuan potassium oxide content is 10% potassium felspar sand double centner, joins in the lining tetrafluoro autoclave of 1000L; The sulfuric acid that adds 700 kilogram 5%; Add 60 kilograms of fluorites, closed reactor.Control 140 ℃ of reacting by heating of temperature 12 hours, sampling, the potassium oxide content of analyzing the sour water reaction solution with the 6400A flame photometer is 1.3%, finishes reaction.Be cooled to room temperature, filter.The filtrate decompression distillation, capable of circulation the applying mechanically of hydrofluoric acid containing sour water distilled out.The solid obtained after evaporate to dryness is exactly 62 kilograms of the soluble potassium salts that extract.With the 6400A flame photometer, analyze, potassium oxide content is 14.8%, and main component is sal enixum, Tai-Ace S 150 and part of sulfuric acid hydrogen potassium.Extraction yield through the present embodiment potassium is 92%.
Embodiment 5
Getting Wangcang County, Sichuan potassium oxide content is 12% potassium felspar sand double centner, joins in the lining tetrafluoro autoclave of 1000L; The sulfuric acid that adds 700 kilogram 5%; Add 50 kilogram of 40% hydrofluoric acid, closed reactor.Control 130 ℃ of reacting by heating of temperature 10 hours, sampling, the potassium oxide content of analyzing the sour water reaction solution with the 6400A flame photometer is 1.5%, finishes reaction.Be cooled to room temperature, filter, filtrate decompression distillation, capable of circulation the applying mechanically of hydrofluoric acid containing sour water distilled out.The solid 51 obtained after evaporate to dryness.With the 6400A flame photometer, analyze, potassium oxide content is 21.5%, and main component is sal enixum, Tai-Ace S 150 and part of sulfuric acid hydrogen potassium.Extraction yield through the present embodiment potassium is 91.7%.
The above; it is only preferably embodiment of the present invention; but protection scope of the present invention is not limited to this; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to replacement or changed according to technical scheme of the present invention and inventive concept thereof, within all should being encompassed in protection scope of the present invention.
Claims (4)
1. the method that an acid system extracts soluble potassium from potassium felspar sand comprises the following steps:
(1) by the potassium felspar sand powder, lower concentration mineral acid, auxiliary agent hydrofluoric acid (HF) or fluorite (CaF
2) directly feed intake, be loaded in airtight lining Monel 400 alloys or lining tetrafluoro autoclave and react;
(2) take out step (1) resultant of reaction, be cooled to room temperature, filter;
(3) filtrate in step (2) is carried out to underpressure distillation, evaporate to dryness, cooled solid are soluble potassium salt.
2. extract the method for soluble potassium according to the described a kind of acid system of right 1 from potassium felspar sand, it is characterized in that, the weight ratio of the potassium felspar sand powder in described step (1), lower concentration mineral acid, hydrofluoric acid or fluorite is 1:5～10:0.5～1.
3. extract the method for soluble potassium according to the described a kind of acid system of right 1 from potassium felspar sand, it is characterized in that, lower concentration acid preferably sulfuric acid (H in described step (1)
2SO
4) and hydrochloric acid (HCl), sulfuric acid (H
2SO
4) concentration is 2～5%, hydrochloric acid (HCl) concentration is 3～8%.
4. extract the method for soluble potassium according to the described a kind of acid system of right 1 from potassium felspar sand, it is characterized in that, the temperature in described step (1) in lining Monel 400 alloys or lining tetrafluoro autoclave is 90～150 ℃, and the reaction times is 5～12 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106348814A (en) * | 2016-08-23 | 2017-01-25 | 贵州远盛钾业科技有限公司 | Method for producing macro-element water-soluble fertilizer by utilizing potassium-containing rocks |
| CN110357116A (en) * | 2018-03-26 | 2019-10-22 | 骆曦明 | A kind of method that potassium albite removes potassium, sodium |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1138567A (en) * | 1996-03-19 | 1996-12-25 | 化学工业部长沙化学矿山设计研究院 | Wetting decomposition process of potash feldspar ore |
| CN102001688A (en) * | 2010-12-01 | 2011-04-06 | 陈锋 | Process for producing potassium sulfate by decomposing potassium feldspar at low temperature with fluorine-containing acid |
| CN103172074A (en) * | 2013-01-17 | 2013-06-26 | 洛阳氟钾科技有限公司 | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization |
-
2013
- 2013-07-26 CN CN2013103176646A patent/CN103420399A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1138567A (en) * | 1996-03-19 | 1996-12-25 | 化学工业部长沙化学矿山设计研究院 | Wetting decomposition process of potash feldspar ore |
| CN102001688A (en) * | 2010-12-01 | 2011-04-06 | 陈锋 | Process for producing potassium sulfate by decomposing potassium feldspar at low temperature with fluorine-containing acid |
| CN103172074A (en) * | 2013-01-17 | 2013-06-26 | 洛阳氟钾科技有限公司 | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization |
Non-Patent Citations (2)
| Title |
|---|
| 唐洪明 等: "酸化体系中长石的稳定性研究", 《天然气工业》 * |
| 薛彦辉 等: "钾长石-萤石-硫酸体系中分解钾长石的探讨", 《化学与生物工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106348814A (en) * | 2016-08-23 | 2017-01-25 | 贵州远盛钾业科技有限公司 | Method for producing macro-element water-soluble fertilizer by utilizing potassium-containing rocks |
| CN110357116A (en) * | 2018-03-26 | 2019-10-22 | 骆曦明 | A kind of method that potassium albite removes potassium, sodium |
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Effective date of registration: 20161027 Address after: 200120 Shanghai city Pudong New Area Lvke Road No. 90 Applicant after: Shanghai Ding Ding Industrial Technology Co., Ltd. Address before: 611400 B District, Xinjin Industrial Park, Xinjin County, Chengdu, Sichuan Applicant before: Chengdu Chemical Co., Ltd. |
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Application publication date: 20131204 |