CN100457692C - Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar - Google Patents
Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar Download PDFInfo
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- CN100457692C CN100457692C CNB2006101560311A CN200610156031A CN100457692C CN 100457692 C CN100457692 C CN 100457692C CN B2006101560311 A CNB2006101560311 A CN B2006101560311A CN 200610156031 A CN200610156031 A CN 200610156031A CN 100457692 C CN100457692 C CN 100457692C
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Abstract
This invention relates to a preparation method of nitrogen, phosphorus and potassium compound (NPK) fertilizer. First mix phosphorus rock powder and potassium feldspar powder by 0.5 to 1.2 of quality, under 150 ~ 250 deg use 20 ~ 50% inorganic acid to immerse for 3 hours, then use the ammonia or carbon ammonium directly neutralize to PH 6 ~ 7, or acid leaching reaction products by dilution, separation and subsequent through ammoniation to PH 6 ~ 7; at last carry out enrichment, granulation and drying to obtain NPK fertilizer that total nutrient not less than 15% or 45%. The preparation method makes acid hydrolysis and calcium, potassium ion exchange be completed simultaneously, in the relatively mild conditions using insoluble, low-grade potassium feldspar to prepare potassium fertilizer. The phosphorus utilization of phosphorus rock powder is not less than 90%, potassium utilization of potassium feldspar not less than 80%.
Description
One, technical field
The present invention relates to a kind of preparation method of chemical fertilizer, particularly the preparation method of multi-component composite fertilizer exactly, is a kind of method for preparing nitrogen-phosphorus-potassium compound fertilizer with potassium felspar sand.
Two, background technology
China's potassium resource is not abundant, soluble potassium resource wretched insufficiency.1.16 hundred million tons of Qinghai sylvite reserves (KCl meter), potassium-rich brine ore bed KCl average grade 1.29%; 2.5 hundred million tons of Lop Nur, Xinjiang sylvite reserves (KCl meter), bittern KCl average grade 1.40%.China's soluble potassium salt reserves per capita only is 1/14 of world average level; And potassium application is to improve the crop quality greatest factor, causes a large amount of import potash fertilizer of having to, and at present, the external interdependency of China's potash fertilizer reaches more than 80%.
The explored water-soluble sylvite in the world mainly concentrates on a few countries such as Canada, Russia, Byelorussia, Germany, Israel, Jordan, though world's sylvite output greater than consumption, Potash Resources has monopoly, can form monopoly price.Therefore, improve China's potash fertilizer degree of self-sufficiency utmost point important meaning is arranged.
China's insoluble low grade potassium ore reserves surpasses 5,000,000,000 t K
2O (rolling over 8,000,000,000 t KCl), and be distributed widely in the agriculture production area.Wherein, based on potassium felspar sand, China's extracting potassium from potash feldspar system potash fertilizer technology development work starts from the fifties end, owing to lack mechanism research, technology development work is made slow progress.Typical at present operational path has: (1) vaporization at high temperature method is with the stove of preparing burden in proportion after the fragmentations such as potassium felspar sand, Wingdale, rhombspar, fluorite and coke.Fire box temperature is up to 1600 ℃, the K that evaporates
2CO in O and the stove
2Effect generates K
2CO
3Shortcoming is that energy consumption is too high, and the potassium yield is on the low side, no economic benefit.(2) high-temperature sintering process, be potassium felspar sand, additive are mixed levigate, fusion roasting in High Temperature Furnaces Heating Apparatus.Temperature is about 1000 ℃, and economic benefit still is difficult to reach a standard, and exists serious high temperature corrosion and lower floor's bits to be difficult to problems such as processing.(3) fluorine decomposition method, be with fluorochemical or fluorine-containing auxiliary agent in inorganic acid medium, in decomposing of potassium feldspar below 200 ℃, because the side reaction product potassium silicofluoride only is dissolved in hydrochloric acid soln, water insoluble, cause the extraction yield of potassium in the non-hydrochloric acid system can be very not high, the highest can only be about 80%.Simultaneously, anti-fluorine etching apparatus difficult quality reaches a standard.(4) microbiological degradation method is to utilize auxiliary material and potassium felspar sand generation biochemical reactions such as microbial bacterial.This method advantage is that flow process is short, three-waste free discharge.But the fecundity of bacterial classification and vitality a little less than, be difficult to survive under field conditions (factors), also need to adopt genetically engineered further to screen and cultivate new bacterial strain.Decomposition rate is slow simultaneously, the time is long, transformation efficiency is low, can not be used for large-scale industrial production.
The applicant has carried out fundamental research to potassium felspar sand, thereby the structure and the character of potassium felspar sand has been had deep understanding.Aluminium in the potassium felspar sand and silicon are all formed the coordination tetrahedron with oxygen, form firm tetrahedral network structure, and its chemical property stabilizer pole is not decomposed by any soda acid except that hydrofluoric acid under the normal temperature.But have bigger space (see figure 1) in the potassium felspar sand structure significantly, under certain conditions, Ca
2+, Na
+Deng the network-modifying ion K that can replace in the potassium felspar sand structure
+Thereby proposed in potassium felspar sand, to put forward the reaction mechanism of potassium with ion exchange method.
At present, nitrogen phosphorus potassium ternary compound fertilizer is mainly formed with formulated such as Repone K by urea, general calcium or fused(calcium magnesium)phosphate, is mixture.Total nutrient (N+P
2O
5+ K
2O) high density is 40%, and middle concentration is 30%, and lower concentration is 25% (GB-15063-94).Generally about 28%.
The Rock Phosphate (72Min BPL) main component is calcium monofluorophosphate (Ca
5(PO
4)
3F), be the main raw material of preparation phosphate fertilizer and phosphoric acid.
Three, summary of the invention
The present invention uses above-mentioned reaction mechanism to change the potassium in the potassium felspar sand into can be absorbed by crop active potassium, its objective is the low-grade potassium felspar sand of development and use, and technical problem to be solved is directly to prepare nitrogen, phosphorus, potassium Nitrogen, Phosphorus and Potassium with potassium felspar sand.
The present invention selects Rock Phosphate (72Min BPL) to be total to acid leaching process with potassium felspar sand.In the acidleach process, mineral acid decomposing phosphate rock stone makes calcium wherein dissociate out, and then displaces the potassium (being ion-exchange) of potassium felspar sand.This process is represented by following chemical equation:
Ca
2++2KAlSi
3O
8→CaAl
2Si
2O
8+2K
++4SiO
2↓
From following formula, as can be seen, in the product of acid-leaching reaction, contain active phosphorus (H
2PO
4 +) and active potassium (K
+), and solution is acid, therefore available ammonia (gas ammonia or liquefied ammonia), ammoniacal liquor or carbon ammonium neutralize, and (also claiming ammonification), to introduce active nitrogen (be ammonium nitrogen NH
4 +), just obtain nitrogen, phosphorus, potassium Nitrogen, Phosphorus and Potassium through concentrated, granulation, drying then.
It can also be seen that to also have by products such as lime feldspar, silicon-dioxide from following formula in the acid-leaching reaction product, these by products are inert, and staying not to influence its stability in the composite fertilizer, execute in the soil and also can not destroy soil.
This preparation method is raw material with the potassium felspar sand, comprise ore fragmentation, pulverizing, mixing, acidleach, concentrate, granulation and drying, difference with the prior art is, rock phosphate powder and feldspar in powder mix, directly carry out ammonification after the acidleach or carry out ammonification through dilution, after separating, described ammonification is neutralized to pH 6～7 with ammonia or ammoniacal liquor or carbon ammonium exactly, concentrates after the ammonification, granulation and drying.
To be exactly rock phosphate powder and feldspar in powder mix the back working concentration mutually with 0.5～1.2 mass ratio is 20～50% (weight percent concentration in described acidleach, mineral acid down together) carries out acid-leaching reaction, liquid-solid ratio is 1～7mL/g breeze, 150～250 ℃ of temperature of reaction, 1～3 hour reaction times.
Preferred rock phosphate powder and feldspar in powder mix mutually with 0.8～1.0 mass ratio, and the mineral acid with 25～45% carries out acidleach, and liquid-solid ratio is 2～5mL/g breeze, 165～230 ℃ of temperature of reaction.
Described mineral acid is selected from phosphoric acid, hydrochloric acid or nitric acid.
Directly carry out ammonification to pH6～7 with ammonia or ammoniacal liquor or carbon ammonium after acid-leaching reaction finishes, concentrate then, granulation and drying, can only obtain the lower concentration Nitrogen, Phosphorus and Potassium of total nutrient 〉=15%, this originates from the diluting effect of lime feldspar, silicon-dioxide.Another kind is to separate before the ammonification to remove lime feldspar, silicon-dioxide etc.Concrete grammar is at first thin up, leaching, make water miscible composition transfer in the solution as far as possible, follow filtering separation, remove precipitations such as lime feldspar, silicon-dioxide, then ammonification or slough portion water after again ammonification to pH 6～7, concentrate at last, granulation and drying, obtain the high concentration ternary composite fertilizer of total nutrient 〉=45%.
This preparation method, achievement based on the laboratory fundamental research, design the technology that under gentle relatively condition, prepares potash fertilizer with potassium felspar sand, and in technology, dexterously the exchange of the acidolysis of Rock Phosphate (72Min BPL) and calcium, potassium ion is integrated in the same system and finishes synchronously, both simplify flow process, initiated the new preparation method of nitrogen, phosphorus, potassium Nitrogen, Phosphorus and Potassium again.This preparation method, the utilization ratio of phosphorus 〉=90% in the Rock Phosphate (72Min BPL), the utilization ratio of potassium 〉=80% in the potassium felspar sand, prepared high-concentration compound fertilizer, total nutrient 〉=45%, more taller than the total nutrient 40% of GB-15063-94 regulation.
Four, description of drawings
Accompanying drawing is a potassium felspar sand tetrahedral network structure synoptic diagram.
The Utopian potassium felspar sand frame of A-shape structure, drawing is perpendicular to axle;
The silica chain that is parallel to axle that the Utopian false four directions of B-ring is constituted.
Five, specific implementation method
1, raw material is prepared
Get the broken respectively back of Rock Phosphate (72Min BPL), potassium felspar sand ball milling, it is standby to cross 80～200 mesh sieves.
Get industrial phosphoric acid content 50～85%, industrial ammonia content 20～27%, standby.
2, acid-leaching reaction
Get rock phosphate powder and feldspar in powder and mix by 0.8～1.0 mass ratio, add industrial phosphoric acid, the control liquid-solid ratio is 2～5mL/g breeze, and acid-leaching reaction is 1～3 hour under 150～250 ℃ of conditions.
3, ammonification
(1) acid-leaching reaction finishes the ammonification of post-treatment industry ammoniacal liquor to pH 6.5, evaporates then, concentrates, granulation, final drying, obtains the Nitrogen, Phosphorus and Potassium of total nutrient 〉=15%.
(2) acid-leaching reaction finishes back thin up, leaching, and filtering separation reclaims filtrate then, sloughs the ammonification of portion water post-treatment industry ammoniacal liquor to pH 6.5, evaporation, concentrates and granulation, and final drying obtains the Nitrogen, Phosphorus and Potassium of total nutrient 〉=45%.
Claims (2)
1, a kind of potassium felspar sand prepares the method for nitrogen-phosphorus-potassium compound fertilizer, with the potassium felspar sand is raw material, comprise fragmentation, pulverizing, mixing, acidleach, concentrate, granulation and drying, it is characterized in that: rock phosphate powder and feldspar in powder by 0.8～1.0 mass ratio mix the back add concentration be 50% phosphoric acid in 165～230 ℃ of following acidleach 1～3 hour, phosphoric acid is pressed 5ml/g
BreezeSolid-to-liquid ratio add; After finishing, acidleach directly is neutralized to pH6～7 with ammonia or ammoniacal liquor or carbon ammonium.
2, method according to claim 1 is characterized in that: acidleach finishes the back thin up, is neutralized to pH6～7 with ammonia or ammoniacal liquor or carbon ammonium after separating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101560311A CN100457692C (en) | 2006-12-31 | 2006-12-31 | Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar |
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|---|---|---|---|
| CNB2006101560311A CN100457692C (en) | 2006-12-31 | 2006-12-31 | Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar |
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|---|---|
| CN100999423A CN100999423A (en) | 2007-07-18 |
| CN100457692C true CN100457692C (en) | 2009-02-04 |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432367A (en) * | 2011-09-21 | 2012-05-02 | 安徽华岳矿物材料有限公司 | Method for preparing mineral potash fertilizer with potassium feldspar |
| CN103274815B (en) * | 2013-05-27 | 2014-11-12 | 隋朋昌 | Preparation method of water-soluble silicon-potassium fertilizer |
| CN103980009B (en) * | 2014-05-26 | 2016-04-13 | 武汉工程大学 | Hydromica barium ion exchange process extracts soluble potassium ion |
| CN105330421A (en) * | 2014-11-15 | 2016-02-17 | 深圳市芭田生态工程股份有限公司 | Method for preparing complex-state mineral element organic liquid fertilizer |
| CN105753588A (en) * | 2016-05-17 | 2016-07-13 | 安徽永冠农业科技有限公司 | Bactericidal insecticidal nitrogen phosphorus and potassium composite fertilizer and preparation method thereof |
| CN105753587A (en) * | 2016-05-17 | 2016-07-13 | 安徽永冠农业科技有限公司 | Nitrogen, phosphorus and potassium compound fertilizer capable of enhancing soil fertility and preparation method of nitrogen, phosphorus and potassium compound fertilizer |
| CN105753589A (en) * | 2016-05-17 | 2016-07-13 | 安徽永冠农业科技有限公司 | Nitrogen, phosphorus and potassium compound fertilizer containing activated carbon and preparation method of nitrogen, phosphorus and potassium compound fertilizer |
| WO2018032066A1 (en) * | 2016-08-17 | 2018-02-22 | Mineração Curimbaba Ltda. | Phosphorus-potassium fertilizer (pk) |
| CN106278480A (en) * | 2016-08-22 | 2017-01-04 | 孙国锋 | A kind of Nutrition Soil planting Caulis et Folium Brassicae capitatae and preparation method thereof |
| CN106631284A (en) * | 2017-01-04 | 2017-05-10 | 山西农业大学 | Preparation method of citrate-soluble potassium inorganic compound fertilizer |
| CN110776363A (en) * | 2019-11-13 | 2020-02-11 | 武汉工程大学 | Compound fertilizer preparation method and product prepared by same |
| CN112898073B (en) * | 2021-01-14 | 2023-01-20 | 襄阳泽东化工集团股份有限公司 | Method for preparing NPK compound fertilizer by using phosphate tailings and potassium feldspar |
| CN112758937B (en) * | 2021-01-14 | 2023-08-01 | 襄阳泽东化工集团有限公司 | Method for preparing potassium fluosilicate and NPK compound fertilizer from associated phosphate-potassium ore |
| CN112745160A (en) * | 2021-01-21 | 2021-05-04 | 瓮福（集团）有限责任公司 | Novel process for preparing NPK compound fertilizer by using phosphogypsum and potassium feldspar |
| CN113184855A (en) * | 2021-04-21 | 2021-07-30 | 武汉工程大学 | Resource comprehensive utilization method of phosphogypsum and potassium feldspar |
| CN113173584A (en) * | 2021-04-21 | 2021-07-27 | 武汉工程大学 | Resource comprehensive utilization method of phosphorus tailings and potassium feldspar |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557781A (en) * | 2004-02-04 | 2004-12-29 | 薛彦辉 | Low temperature decomposition method for potassium feldspar |
| CN1793065A (en) * | 2005-11-28 | 2006-06-28 | 四川大学 | Process for producing slow releasing silicon potassium compound fertilizer by potassium feldspar |
-
2006
- 2006-12-31 CN CNB2006101560311A patent/CN100457692C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557781A (en) * | 2004-02-04 | 2004-12-29 | 薛彦辉 | Low temperature decomposition method for potassium feldspar |
| CN1793065A (en) * | 2005-11-28 | 2006-06-28 | 四川大学 | Process for producing slow releasing silicon potassium compound fertilizer by potassium feldspar |
Non-Patent Citations (2)
| Title |
|---|
| 钾长石与磷矿共酸浸提钾过程实验研究. 韩效钊，胡波，肖正辉等.化工矿物与加工，第9期. 2005 |
| 钾长石与磷矿共酸浸提钾过程实验研究. 韩效钊，胡波，肖正辉等.化工矿物与加工，第9期. 2005 * |
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| CN100999423A (en) | 2007-07-18 |
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Assignee: Anhui Jindihao Fertilizer Industry Co., Ltd. Assignor: Hefei University of Technology Contract fulfillment period: 2009.6.9 to 2014.6.10 contract change Contract record no.: 2009340000268 Denomination of invention: Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar Granted publication date: 20090204 License type: Exclusive license Record date: 2009.9.4 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.6.9 TO 2014.6.10; CHANGE OF CONTRACT Name of requester: ANHUI JINDIHAO FERTILIZER CO., LTD. Effective date: 20090904 |
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Granted publication date: 20090204 Termination date: 20161231 |