CN103539163B - Utilize the technique of potassium felspar sand preparing potassium sulfate - Google Patents
Utilize the technique of potassium felspar sand preparing potassium sulfate Download PDFInfo
- Publication number
- CN103539163B CN103539163B CN201310527135.9A CN201310527135A CN103539163B CN 103539163 B CN103539163 B CN 103539163B CN 201310527135 A CN201310527135 A CN 201310527135A CN 103539163 B CN103539163 B CN 103539163B
- Authority
- CN
- China
- Prior art keywords
- potassium
- leaching
- felspar sand
- reaction
- silicofluoride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Fertilizers (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention provides the technique utilizing potassium felspar sand preparing potassium sulfate, comprise the following steps: (1) react: by potassium felspar sand, fluorite, Neutral ammonium fluoride, 98% sulfuric acid fully mix rear reaction; (2) gas absorption: gas reaction produced introduces dedusting in dust removal filter, to be passed into successively in I and II absorption tower and to be absorbed by absorption liquid after dust removal and filtration; (3) leaching of reaction residues: solid residue is proceeded to leaching groove by discharging spiral, leaches with dilution heat of sulfuric acid; (4) preparation of potassium silicofluoride: add silicate fluoride solution in leaching liquid, obtained potassium silicofluoride powder; (5) preparation of potassium sulfate: potassium silicofluoride powder and the vitriol oil drop in calcining furnace, after reaction, residue dissolves, filters and obtain potassium product to filtrate recrystallization by residue clear water.Present invention achieves the transformation of insoluble sylvite to soluble potassium salt, prepared highly purified potassium sulfate, solved the problem of China's soluble potassium inadequate resource.
Description
Technical field
The present invention relates to potassium feldspar decomposition comprehensive utilization technique, be specifically related to a kind of technique utilizing potassium felspar sand preparing potassium sulfate.
Background technology
Use fertilizer to be step indispensable in modern agricultural production, in existing fertilizer, potassium nutrition element occupies very important position.Shi Ge large agricultural country of China, because China's soluble potassium resource is extremely poor, be difficult to meet domestic needs, China is proportion of N and K fertilizer numerous imbalances on agricultural fertilizer.But China's insoluble potassium resource is a lot, especially potash feldspar ore reserves are extremely abundant, mainly be distributed in 19 provinces and regions such as Yunnan, Guizhou, Sichuan, Hunan, Hubei, Henan, Anhui, Jiangxi, Shandong and Xinjiang, therefore, how utilizing potassium felspar sand to manufacture potash fertilizer is problem demanding prompt solution.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, thus the technique utilizing potassium felspar sand preparing potassium sulfate is provided.
To achieve these goals, the technical solution adopted in the present invention is: the technique utilizing potassium felspar sand preparing potassium sulfate, comprises the following steps:
(1) react: after potassium felspar sand, fluorite, Neutral ammonium fluoride, the vitriol oil fully being mixed, 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, the vitriol oil is the sulfuric acid of 98%, 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;
(2) gas absorption: gas reaction produced introduces dedusting in dust removal filter, to pass into successively after dust removal and filtration in I and II absorption tower and to be absorbed by absorption liquid, generate white precipitate and silicate fluoride solution, through centrifugation, washing and dry obtained white carbon black product, gained filtrate is silicate fluoride solution; Wherein absorption liquid is the aqueous ethanolic solution of 10 ~ 30%; Reaction principle is: 3SiF
4+ 2H
2o=2H
2siF
6+ SiO
2↓;
(3) leaching of reaction residues: reacted solid residue in described converter reactor is proceeded to leaching groove by discharging spiral, at 90 ~ 110 DEG C, with the dilution heat of sulfuric acid leaching that volume fraction is 8 ~ 10%, then filtration is carried out to the solution after leaching and obtain leaching liquid;
(4) preparation of potassium silicofluoride: leaching liquid is got in potassium silicofluoride reactor through pump and regulates temperature at 55 ~ 65 DEG C, add silicate fluoride solution obtained in step (2) according to stoichiometric relation and generate potassium silicofluoride precipitation, silicofluoric acid excessive 20 ~ 100%, through ageing, then through Filter Press, washing also dry obtained potassium silicofluoride powder;
(5) preparation of potassium sulfate: potassium silicofluoride powder obtained in step (4) and the vitriol oil are dropped in calcining furnace, potassium silicofluoride and sulfuric acid mole ratio be 1:1.05 ~ 1.1,0.5 ~ 1h is reacted at 150 ~ 300 DEG C, the gas produced passes into I and II absorption tower successively and absorbs, after reaction, the main component of residue is potassium sulfate and contains a small amount of silicon-dioxide, with clear water, residue is dissolved, then filter and potassium product is obtained to filtrate recrystallization.
Based on above-mentioned, in step (2), it is cyclic absorption process that gas leads in I and II absorption tower the process carrying out absorbing successively.
Based on above-mentioned, with the solids manufacture aerated bricks filtered out in step (3).
The present invention utilizes the technique of potassium felspar sand preparing potassium sulfate, compared with prior art has following main advantage:
1. the present invention adopts the technique of low temperature semidrying decomposing of potassium feldspar, and temperature of reaction is at 180 ~ 250 DEG C, and compared with pyroprocess decomposing of potassium feldspar, reaction conditions is gentle, lower to the requirement of equipment.
2. the present invention is directed to the problem that potassium element that potassium felspar sand contains belongs to insoluble potassium resource, a kind of fluorine-containing auxiliary agent low-temperature decomposing of potassium feldspar is proposed, by to dissolve and sylvite extracts separately by the method adding silicate fluoride solution, react at 150 ~ 300 DEG C further, pass into the vitriol oil afterwards to obtain potassium sulfate and obtain solid sulphuric acid potassium by crystallization, achieve the transformation of insoluble sylvite to soluble potassium salt, prepare highly purified potassium sulfate, provide a kind of new approaches, solve the problem of China's soluble potassium inadequate resource.Production process produces without the three wastes, and energy consumption is low, output is high, the rate of recovery is high, achieves production serialization, and the effective constituent of potassium felspar sand have also been obtained sufficient utilization.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the present invention utilizes potassium felspar sand preparing potassium sulfate.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Utilize the embodiment of the technique of potassium felspar sand preparing potassium sulfate
Embodiment 1
As shown in Figure 1, comprise the following steps:
(1) react: 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;
(2) gas absorption: gas reaction produced introduces dedusting in dust removal filter, to pass into successively after dust removal and filtration in I and II absorption tower and to be absorbed by absorption liquid, generate white precipitate and silicate fluoride solution, through centrifugation, washing and dry obtained white carbon black product, gained filtrate is silicate fluoride solution; Wherein absorption liquid is the aqueous ethanolic solution of 10 ~ 30%; Reaction principle is: 3SiF
4+ 2H
2o=2H
2siF
6+ SiO
2↓;
(3) leaching of reaction residues: reacted solid residue in described converter reactor is proceeded to leaching groove by discharging spiral, at 100 DEG C, is the dilution heat of sulfuric acid leaching of 10% by volume fraction, then carries out filtration to the solution after leaching and obtain leaching liquid;
(4) preparation of potassium silicofluoride: leaching liquid is got in potassium silicofluoride reactor through pump and regulates temperature at 60 DEG C, add silicate fluoride solution obtained in step (2) according to stoichiometric relation and generate potassium silicofluoride precipitation, silicofluoric acid excessive 20 ~ 100%, through ageing, then through Filter Press, washing also dry obtained potassium silicofluoride powder;
(5) preparation of potassium sulfate: potassium silicofluoride powder obtained in step (4) and the vitriol oil are dropped in calcining furnace, potassium silicofluoride and sulfuric acid mole ratio be 1:1.1,0.5 ~ 1h is reacted at 150 ~ 300 DEG C, the gas produced passes into I and II absorption tower successively and absorbs, after reaction, the main component of residue is potassium sulfate and contains a small amount of silicon-dioxide, with clear water, residue is dissolved, then filter and potassium product is obtained to filtrate recrystallization.
The present invention utilizes the technique of potassium felspar sand preparing potassium sulfate to adopt the technique of low temperature semidrying decomposing of potassium feldspar, and compared with pyroprocess decomposing of potassium feldspar, reaction conditions is gentle, lower to the requirement of equipment; The potassium element contained potassium felspar sand belongs to the problem of insoluble potassium resource, a kind of fluorine-containing auxiliary agent low-temperature decomposing of potassium feldspar is proposed, by to dissolve and sylvite extracts separately by the method adding silicate fluoride solution, react at 150 ~ 300 DEG C further, pass into dilute sulphuric acid afterwards to obtain potassium sulfate and obtain solid sulphuric acid potassium by crystallization, achieve the transformation of insoluble sylvite to soluble potassium salt, prepare highly purified potassium sulfate, provide a kind of new approaches, solve the problem of China's soluble potassium inadequate resource.Production process produces without the three wastes, and energy consumption is low, output is high, the rate of recovery is high, achieves production serialization, and the effective constituent of potassium felspar sand have also been obtained sufficient utilization.
Embodiment 2
As different from Example 1, in step (2), it is cyclic absorption process that gas leads in I and II absorption tower the process carrying out absorbing successively, and object is the concentration improving constantly silicate fluoride solution.
Embodiment 3
With above-described embodiment unlike, with the solids manufacture aerated bricks filtered out in step (3).
In other embodiments of the invention, with above-described embodiment unlike, in step (1), (1) temperature of reaction can choose 180 DEG C, 200 DEG C or 250 DEG C as required, potassium felspar sand, fluorite, Neutral ammonium fluoride, 98% sulfuric acid mass ratio can be chosen for 1:0.3:1.12:1.6 as required, 1:0.4:1.4:1.7 or 1:0.5:1.73:1.8; In step (2), absorption liquid can choose the aqueous ethanolic solution of 10% as required, the aqueous ethanolic solution of 20% or the aqueous ethanolic solution of 30%; In step (3), temperature can also as required at 90 DEG C or 110 DEG C etc., the volume fraction of dilution heat of sulfuric acid can also choose 8% or 9% etc. as required, in step (4), can adjust the temperature to 55 DEG C or 65 DEG C etc. as required, silicofluoric acid can as required excessive 20%, 50% even 100%; In step 5, temperature of reaction can be 150 DEG C, 250 DEG C or 300 DEG C, and the reaction times can select 0.50h, 7h or 1h, potassium silicofluoride and sulfuric acid mole ratio can choose 1:1.05 or 1:1.08 etc. as required.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (3)
1. utilize the technique of potassium felspar sand preparing potassium sulfate, it is characterized in that comprising the following steps:
(1) react: 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;
(2) gas absorption: gas reaction produced introduces dedusting in dust removal filter, to pass into successively after dust removal and filtration in I and II absorption tower and to be absorbed by absorption liquid, generate white precipitate and silicate fluoride solution, through centrifugation, washing and dry obtained white carbon black product, gained filtrate is silicate fluoride solution; Wherein absorption liquid is the aqueous ethanolic solution of 10 ~ 30%; Reaction principle is: 3SiF
4+ 2H
2o=2H
2siF
6+ SiO
2↓;
(3) leaching of reaction residues: reacted solid residue in described converter reactor is proceeded to leaching groove by discharging spiral, at 90 ~ 110 DEG C, with the dilution heat of sulfuric acid leaching that volume fraction is 8 ~ 10%, then filtration is carried out to the solution after leaching and obtain leaching liquid;
(4) preparation of potassium silicofluoride: leaching liquid is got in potassium silicofluoride reactor through pump and regulates temperature at 55 ~ 65 DEG C, add silicate fluoride solution obtained in step (2) according to stoichiometric relation and generate potassium silicofluoride precipitation, silicofluoric acid excessive 20 ~ 100%, through ageing, then through Filter Press, washing also dry obtained potassium silicofluoride powder;
(5) preparation of potassium sulfate: potassium silicofluoride powder obtained in step (4) and the vitriol oil are dropped in calcining furnace, potassium silicofluoride and sulfuric acid mole ratio be 1:1.05 ~ 1.1,0.5 ~ 1h is reacted at 150 ~ 300 DEG C, the gas produced passes into I and II absorption tower successively and absorbs, after reaction, the main component of residue is potassium sulfate and contains a small amount of silicon-dioxide, with clear water, residue is dissolved, then filter and potassium product is obtained to filtrate recrystallization.
2. the technique utilizing potassium felspar sand preparing potassium sulfate according to claim 1, is characterized in that: in step (2), and it is cyclic absorption process that gas leads in I and II absorption tower the process carrying out absorbing successively.
3. the technique utilizing potassium felspar sand preparing potassium sulfate according to claim 1 and 2, is characterized in that: with the solids manufacture aerated bricks filtered out in step (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310527135.9A CN103539163B (en) | 2013-10-31 | 2013-10-31 | Utilize the technique of potassium felspar sand preparing potassium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310527135.9A CN103539163B (en) | 2013-10-31 | 2013-10-31 | Utilize the technique of potassium felspar sand preparing potassium sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103539163A CN103539163A (en) | 2014-01-29 |
| CN103539163B true CN103539163B (en) | 2016-03-02 |
Family
ID=49963085
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310527135.9A Active CN103539163B (en) | 2013-10-31 | 2013-10-31 | Utilize the technique of potassium felspar sand preparing potassium sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103539163B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439167A (en) * | 2015-11-29 | 2016-03-30 | 洛阳绿仁环保设备有限公司 | Method for preparing 3A molecular sieve from potassium feldspar |
| CN105439160A (en) * | 2015-11-29 | 2016-03-30 | 洛阳绿仁环保设备有限公司 | Method for preparing potassium silicate from potassium feldspar |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB135545A (en) * | ||||
| CN1118333A (en) * | 1994-09-09 | 1996-03-13 | 林延芳 | Process for extracting soluble non-sulfur potassium salt from feldspar |
| CN1146982A (en) * | 1995-05-04 | 1997-04-09 | 贺觉德 | Process for producing potassium sulfate and its by-product using potassium ore |
| CN1259487A (en) * | 1998-11-09 | 2000-07-12 | 裴敬 | Technology of preparing potassium sulfate using leopoldite |
| CN101704687A (en) * | 2009-09-28 | 2010-05-12 | 陈锋 | Method for producing potassium sulphate by decomposing potassium feldspar at low temperature |
| 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
- 2013-10-31 CN CN201310527135.9A patent/CN103539163B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB135545A (en) * | ||||
| CN1118333A (en) * | 1994-09-09 | 1996-03-13 | 林延芳 | Process for extracting soluble non-sulfur potassium salt from feldspar |
| CN1146982A (en) * | 1995-05-04 | 1997-04-09 | 贺觉德 | Process for producing potassium sulfate and its by-product using potassium ore |
| CN1259487A (en) * | 1998-11-09 | 2000-07-12 | 裴敬 | Technology of preparing potassium sulfate using leopoldite |
| CN101704687A (en) * | 2009-09-28 | 2010-05-12 | 陈锋 | Method for producing potassium sulphate by decomposing potassium feldspar at low temperature |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103539163A (en) | 2014-01-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103172074B (en) | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization | |
| CN103539157B (en) | The technique of fluorine resource is reclaimed from potassium feldspar decomposition residue | |
| CN104030328B (en) | The method of active porous shape earth silicon material is prepared with serpentine extraction magnesium oxide | |
| CN107089673A (en) | Method for preparing lithium carbonate by two-stage conversion of lithium ore | |
| CN102424412B (en) | Method of producing alumina from fly ash | |
| CN104003443B (en) | A kind of method adding JZPD capsule ammonium meta-vanadate | |
| CN103011272A (en) | Method for concentrating and purifying titanium dioxide waste acid by using complex acid | |
| CN101607834A (en) | Utilize potassium-bearing mineral, phosphogypsum and high sulphur coal to prepare the method for potash fertilizer and co-producing sulfuric acid | |
| CN101857919A (en) | Method for preparing lead nitrate and lead oxide by using lead plaster of waste lead accumulator | |
| CN103539132B (en) | The method of Neutral ammonium fluoride is reclaimed from potassium felspar sand gas phase adsorption liquid | |
| CN103626208A (en) | Preparation method for high-purity lithium fluoride by taking lithium hexafluorophosphate as raw material | |
| CN104805299A (en) | Method for preparing lithium battery electrode materials LiFePO4 and Li4Ti5O12 from vanadium extraction slag | |
| CN103213991B (en) | Electronic-grade mixing waste acidity recovery and recycle utilization | |
| CN103539163B (en) | Utilize the technique of potassium felspar sand preparing potassium sulfate | |
| CN114014294B (en) | Method for preparing lithium iron phosphate by using pyrite and lithium iron phosphate material | |
| CN101928022B (en) | Method for preparing battery grade lithium fluoride | |
| CN107902631A (en) | One kind utilizes hot carbon reduction ardealite coupling thermal activation potash feldspar ore CO2The method of co-production sulfur dioxide and potassium sulfate | |
| CN103224246B (en) | Chemical gypsum-to-ammonium sulfate reaction slurry concentration, waste heat recovery and waste ammonia recovery method | |
| CN104016357B (en) | A kind of manganese slag for comprehensive utilizes the method for producing industrial chemicals | |
| CN103880630B (en) | A kind of scrap lead cream is used to prepare high-purity lead acetate and the method for nanometer Hydrocerussitum (Ceruse) | |
| CN115010091B (en) | Impurity removal method for hydrogen fluoride, purification method for hydrogen fluoride and purification device for hydrogen fluoride | |
| CN105803187A (en) | Microwave-assisted decomposition method for Baotou mixed rare earth concentrates | |
| CN103539166A (en) | Method for preparing potassium nitrate by use of potassium feldspar | |
| CN104017998B (en) | A kind of manganese slag for comprehensive Application way | |
| CN107416845A (en) | A kind of method that potassium feldspar produces white silica gel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| CB02 | Change of applicant information |
Address after: 471400, Luoyang, Henan, Songxian province township industrial agglomeration area Luoyang potassium fluoride technology joint-stock company Applicant after: LUOYANG POTASSIUM FLUORIDE TECHNOLOGY CO.,LTD. Address before: 471400, Henan, Luoyang province Songxian meal slope Township Industrial Agglomeration Applicant before: Luoyang Fluorine and Potassium Technology Co.,Ltd. Address after: 471400, Henan, Luoyang province Songxian meal slope Township Industrial Agglomeration Applicant after: Luoyang Fluorine and Potassium Technology Co.,Ltd. Address before: 471400, Luoyang, Songxian, Henan province Township Po Industrial Agglomeration Area Luoyang fluorine potassium Technology Co., Ltd. Applicant before: Luoyang Fluoride & Potassium Technology Co.,Ltd. |
|
| COR | Change of bibliographic data | ||
| GR01 | Patent grant |