CN103420402A - Method for extracting soluble potassium from potassium feldspar through alkaline process - Google Patents
Method for extracting soluble potassium from potassium feldspar through alkaline process Download PDFInfo
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- CN103420402A CN103420402A CN2013103176839A CN201310317683A CN103420402A CN 103420402 A CN103420402 A CN 103420402A CN 2013103176839 A CN2013103176839 A CN 2013103176839A CN 201310317683 A CN201310317683 A CN 201310317683A CN 103420402 A CN103420402 A CN 103420402A
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Abstract
The invention discloses a method for extracting soluble potassium from potassium feldspar through the alkaline process. The method comprises the following steps: directly feeding potassium feldspar smashed particles, a potassium hydroxide auxiliary agent and deionized water as per a certain proportion, placing the potassium feldspar smashed particles, the potassium hydroxide auxiliary agent and the deionized water into carbon steel reaction kettle with a condenser, taking out the obtained product after reaction; cooling the obtained product until the temperature of the product reaches indoor temperature, adding acid with low concentration or introducing carbon dioxide gas, neutralizing and filtering, performing reduced pressure distillation on filter liquor, so as to obtain soluble sylvine being the solid obtained after the filter liquor is dried. According to the invention, strong alkali is adopted as the auxiliary agent, the internal structure of the potassium feldspar is effectively destroyed under the condition of low temperature of less than or equal to 120 DEG C, the extraction efficiency of soluble potassium is improved, and the productivity reaches 95% above; the acid with low concentration or carbon dioxide is used for neutralizing the filter liquor, filter residues can be taken as white cement raw materials, and water generated after the distillation of the filter liquor can recycled and used mechanically; besides, the technology has the advantages of simple process, low temperature, less environmental pollution and high extraction efficiency, and the practical application and industrialization prospect is excellent.
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 alkaline process and extract the method for soluble potassium from potassium felspar sand.
Background technology
China's soluble potassium resource is seriously rare, main dependence on import.Yet, refractory potassic mine resource but reserves is abundant, 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, there is important economy and strategic importance.
China's more typical soluble potassium extraction process at present has: (1) vaporization at high temperature method, will after the fragmentations such as potassium felspar sand, calcium oxide, fluorite, enter in proportion stove, and rely on the K produced under hot conditions
2O and CO
2, generate K
2CO
3, this kind of method complex process, seriously polluted.(2) fluorine solution, utilize the mineral acid of fluorochemical, and, in decomposing of potassium feldspar below 200 ℃, this process reaction product potassium silicofluoride is water insoluble, and, the fluoric acid serious corrosion.
In soluble potassium Study on extraction process, the researcher of China is also obtained some progress, but still has significant limitation, main as follows: (1) Chinese patent ZL95104123.1, and with tensio-active agent, CaO, CaSO
4As auxiliary agent, at 200～400 ℃ of high temperature, under the hydrothermal condition of 30～70atm high pressure, react 100min, decomposing of potassium feldspar, K
2O extraction rate reached 90%, this kind of severe reaction conditions, need high temperature and high pressure environment, and equipment requirements is high; (2) Chinese patent ZL01100474.6, take potassium felspar sand: CaO: water is the proportioning of 1:0.8～1:2～6, under the hydrothermal condition of 130～250 ℃ of High Temperature High Pressure, reacts 5～24h decomposing of potassium feldspar, K
2O extraction rate reached 62%, the extraction yield that this patent relates to is lower, and actual application ability is poor; (3) Chinese patent ZL01100475.4, take potassium felspar sand: CaO: gypsum: water is the proportioning of 1:0.8～1:0.2～0.25:2～6, at 130～250 ℃, reacts 5～24h decomposing of potassium feldspar, K under the hydrothermal condition of high pressure
2O extraction rate reached 75%, the soluble potassium extraction process that this patent relates to, extraction yield is lower, though have certain using value, wastage of material is larger.
The applicant has carried out long-term fundamental research to potassium felspar sand, and structure and the physico-chemical property of potassium felspar sand had to comparatively deep understanding.Potassium felspar sand is mainly the aluminum potassium silicate crystallization, and its chemical property is very stable, under normal temperature, is insoluble in hydrochloric acid, and the acid such as sulfuric acid, only have hydrofluoric acid, and silicofluoric acid and highly basic can destroy the stable lattice of aluminum potassium silicate.The existing low-temperature alkaline of China dissolves the potassium extracted in potassium felspar sand and only is confined to the laboratory study stage, because cost is high, can't be applied to actual production.
Summary of the invention
The present invention is directed to existing soluble potassium extraction process, especially there is above-mentioned deficiency in the method for low temperature rapid extraction soluble potassium, provides that a kind of technique is simple, good product quality, extraction yield alkaline process high, good in economic efficiency, non-environmental-pollution 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 alkaline process extracts soluble potassium from potassium felspar sand comprises the following steps:
(1) potassium felspar sand particle, auxiliary agent highly basic, deionized water are directly fed intake, be loaded on band water cooler carbon steel reaction kettle for reaction;
(2) resultant of taking-up step (1) is cooled to room temperature, adds lower concentration acid or passes into carbon dioxide, neutralizes and filters;
(3) filtrate in step (2) is carried out to underpressure distillation, the solid after evaporate to dryness is soluble potassium salt.
The present invention, on the basis of technique scheme, has done following improvement.
Preferentially, the weight ratio of the potassium felspar sand particle in described step (1) or powder, potassium hydroxide auxiliary agent and deionized water is 1:5～10:15～20.
Preferentially, the optional sodium hydroxide of auxiliary agent highly basic, calcium hydroxide or potassium hydroxide in described step (1), preferably potassium hydroxide.
Preferentially, in described step (1), with the temperature in water cooler carbon steel reactor, be 105～115 ℃, reflux time is 2～6 hours.
There is above-mentioned deficiency in the method that the present invention is directed to existing low temperature rapid extraction soluble potassium, a kind of novel process is proposed, its beneficial effect is: alkaline process of the present invention extracts soluble potassium and adopts potassium hydroxide as auxiliary agent, be no more than under the cold condition of 120 ℃, effectively destroyed the internal structure of potassium felspar sand, promoted the extraction yield of soluble potassium, productive rate reaches more than 95%; With lower concentration acid or carbonic acid gas neutralization filtrate, be converted into soluble potassium salt, filter residue can be used as the white cement raw material, and the water that filtrate distills out is capable of circulation to be applied mechanically; The soluble potassium extraction process the present invention relates to has that technique is simple, low temperature, low in the pollution of the environment, extraction yield advantages of higher, and speed of reaction is fast, and low for equipment requirements, practical application and industrial prospect are good.
The accompanying drawing explanation
Fig. 1 is that a kind of alkaline process 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 potassium felspar sand raw ore Mechanical Crushing to particle, potassium felspar sand particle, potassium hydroxide auxiliary agent and deionized water be by weight directly feeding intake for 1:5～10:15～20, and the band condenser carbon steel reactor that to be placed in temperature be 105～115 ℃, react taking-up after 2～6 hours, resultant is cooled to room temperature, add lower concentration acid or pass into carbon dioxide, be neutralized to neutral and filter filtrate low-temperature distillation 3～5 hours, cooling 0.5～1h, can obtain soluble powder sylvite.
The method of with four embodiment, a kind of alkaline process of the present invention being extracted to soluble potassium from potassium felspar sand below is described in further detail.
Embodiment 1
Taking Xuyong County, Sichuan potassium oxide content is 11% potassium felspar sand double centner, join in the band condenser carbon steel reactor of 1000L, 800 kilograms of the rare potassium hydroxide solutions that adds the self-produced potassium hydroxide of Chengdu chemical inc and water to be made into (potassium oxide content is 2.5%), be warming up to backflow, under reflux state, reaction is 4 hours, sampling, be 3.8% with the potassium oxide content of 6400A flame photometer analytical reaction liquid, finishes reaction.Be cooled to room temperature, under stirring, pass into carbonic acid gas, when PH is 10, stop passing into carbonic acid gas, filter.The filtrate decompression distillation, the water distilled out is capable of circulation to be applied mechanically, and obtains the solid of 52.3 kilograms after evaporate to dryness, and main component is salt of wormwood.With the 6400A flame photometer, analyze, potassium oxide content is 38.1%, and the potassium extraction yield is 95.5%.
Embodiment 2
Getting Wangcang County, Sichuan potassium oxide content is 13% potassium felspar sand double centner, join in the band condenser carbon steel reactor of 1000L, 700 kilograms of the rare potassium hydroxide solutions that adds the self-produced potassium hydroxide of Chengdu chemical inc and water to be made into (potassium oxide content is 3%), be warming up to backflow, under reflux state, reaction is 5 hours, sampling is 4.8% with the potassium oxide content of 6400A flame photometer analytical reaction liquid, finishes reaction.Be cooled to room temperature, stir, regulating PH with 10% dilute hydrochloric acid is 7, filters.The filtrate decompression distillation, the water distilled out is capable of circulation to be applied mechanically, and obtains the solid of 65 kilograms after evaporate to dryness, and main component is Repone K.With the 6400A flame photometer, analyze, potassium oxide content is 50.6%, and the potassium extraction yield is 96.8%.
Embodiment 3
Getting Xuyong County, Sichuan potassium oxide content is 13% potassium felspar sand double centner, join in the band condenser carbon steel reactor of 1000L, 800 kilograms of the rare potassium hydroxide solutions that adds the self-produced potassium hydroxide of Chengdu chemical inc and water to be made into (potassium oxide content is 3%), be warming up to backflow, under reflux state, reaction is 6 hours, sampling is 4.5% with the potassium oxide content of 6400A flame photometer analytical reaction liquid, finishes reaction.Be cooled to room temperature, stir, regulating PH with 20% dilute sulphuric acid is 7, filters.The filtrate decompression distillation, the water distilled out is capable of circulation to be applied mechanically, and obtains the solid of 112 kilograms after evaporate to dryness, and main component is vitriolate of tartar.With the 6400A flame photometer, analyze, potassium oxide content is 31.8%, and the potassium extraction yield is 96.2%.
Embodiment 4
Getting Wangcang County, Sichuan potassium oxide content is 12% potassium felspar sand double centner, join in the band condenser carbon steel reactor of 1000L, 600 kilograms of the rare potassium hydroxide solutions that adds the self-produced potassium hydroxide of Chengdu chemical inc and water to be made into (potassium oxide content is 3.5%), be warming up to backflow, under reflux state, reaction is 6 hours, sampling is 5.4% with the potassium oxide content of 6400A flame photometer analytical reaction liquid, finishes reaction, is cooled to room temperature.Pass into carbonic acid gas under stirring, when PH is 10, stop passing into carbonic acid gas, filter.The filtrate decompression distillation, the water distilled out is capable of circulation to be applied mechanically, and obtains the solid of 78 kilograms after evaporate to dryness, and main component is salt of wormwood.With the 6400A flame photometer, analyze, potassium oxide content is 40.5%, and the potassium extraction yield is 95.8%.
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 alkaline process extracts soluble potassium from potassium felspar sand comprises the following steps:
(1) potassium felspar sand particle, auxiliary agent highly basic, deionized water are directly fed intake, be loaded on band water cooler carbon steel reaction kettle for reaction;
(2) resultant of taking-up step (1) is cooled to room temperature, adds lower concentration acid or passes into carbon dioxide, neutralizes and filters;
(3) filtrate in step (2) is carried out to underpressure distillation, the solid after evaporate to dryness is soluble potassium salt.
2. extract the method for soluble potassium according to the described a kind of alkaline process of right 1 from potassium felspar sand, it is characterized in that, the weight ratio of the potassium felspar sand particle in described step (1), auxiliary agent highly basic and deionized water is 1:5～10:15～20.
3. extract the method for soluble potassium according to the described a kind of alkaline process of right 1 from potassium felspar sand, it is characterized in that, the optional sodium hydroxide of auxiliary agent highly basic, calcium hydroxide or potassium hydroxide in described step (1), preferably potassium hydroxide.
4. extracting the method for soluble potassium according to the described a kind of alkaline process of right 1 from potassium felspar sand, it is characterized in that, is 105～115 ℃ with the temperature in water cooler carbon steel reactor in described step (1), and the reaction times is 2～6 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819228A (en) * | 2014-02-26 | 2014-05-28 | 化工部长沙设计研究院 | Method for preparing potash fertilizer and alumina silicate from potash feldspar |
| CN103864496A (en) * | 2014-02-26 | 2014-06-18 | 化工部长沙设计研究院 | Technology for preparing potash fertilizer with potash feldspar |
| CN107337216A (en) * | 2017-07-18 | 2017-11-10 | 昊青薪材（北京）技术有限公司 | A kind of method that potassium feldspar hydro-thermal alkaline process prepares potassium hydroxide |
| CN108238832A (en) * | 2016-12-26 | 2018-07-03 | 中国科学院过程工程研究所 | A kind of method that alkali activation potassium feldspar prepares soluble potassium and calcium silicates soil conditioner |
| CN108439431A (en) * | 2018-03-22 | 2018-08-24 | 滁州方大矿业发展有限公司 | A kind of method that potassium feldspar hydro-thermal alkaline process prepares potassium hydroxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1118333A (en) * | 1994-09-09 | 1996-03-13 | 林延芳 | Process for extracting soluble non-sulfur potassium salt from feldspar |
| CN102408256A (en) * | 2011-08-24 | 2012-04-11 | 烟台大学 | Method for quickly extracting soluble potassium at low temperature |
| CN102557050A (en) * | 2011-12-20 | 2012-07-11 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
-
2013
- 2013-07-26 CN CN2013103176839A patent/CN103420402A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1118333A (en) * | 1994-09-09 | 1996-03-13 | 林延芳 | Process for extracting soluble non-sulfur potassium salt from feldspar |
| CN102408256A (en) * | 2011-08-24 | 2012-04-11 | 烟台大学 | Method for quickly extracting soluble potassium at low temperature |
| CN102557050A (en) * | 2011-12-20 | 2012-07-11 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819228A (en) * | 2014-02-26 | 2014-05-28 | 化工部长沙设计研究院 | Method for preparing potash fertilizer and alumina silicate from potash feldspar |
| CN103864496A (en) * | 2014-02-26 | 2014-06-18 | 化工部长沙设计研究院 | Technology for preparing potash fertilizer with potash feldspar |
| CN103819228B (en) * | 2014-02-26 | 2016-03-09 | 化工部长沙设计研究院 | A kind of method utilizing potassium felspar sand to prepare potash fertilizer and pure aluminium silicate |
| CN103864496B (en) * | 2014-02-26 | 2016-03-09 | 化工部长沙设计研究院 | The technique of potash fertilizer prepared by a kind of potassium felspar sand |
| CN108238832A (en) * | 2016-12-26 | 2018-07-03 | 中国科学院过程工程研究所 | A kind of method that alkali activation potassium feldspar prepares soluble potassium and calcium silicates soil conditioner |
| CN108238832B (en) * | 2016-12-26 | 2021-06-01 | 中国科学院过程工程研究所 | Method for preparing soluble potassium and calcium silicate soil conditioner by alkali-activated potassium feldspar |
| CN107337216A (en) * | 2017-07-18 | 2017-11-10 | 昊青薪材（北京）技术有限公司 | A kind of method that potassium feldspar hydro-thermal alkaline process prepares potassium hydroxide |
| CN108439431A (en) * | 2018-03-22 | 2018-08-24 | 滁州方大矿业发展有限公司 | A kind of method that potassium feldspar hydro-thermal alkaline process prepares potassium hydroxide |
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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 |