CN104744175B - The method that nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals - Google Patents
The method that nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals Download PDFInfo
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Abstract
The invention discloses a kind of method that utilization phosphorus potassium associated minerals produce nitrogen-phosphorus-potassium compound fertilizer, using phosphorus potassium associated minerals as raw material, mixed with sulfuric acid, fluoride auxiliary agent to reactor, heat and reacted successively in the case where reactor carries pressure and condition of negative pressure, after the completion of reaction, bottoms is filtered, gained filtrate adjusts pH to 6.5~8.0 with ammoniacal liquor, again through evaporation, crystallization, granulation, high-concentration compound N-P-K fertilizer is obtained；Gained filter residue adjusts pH to 6.5~8.0 with ammoniacal liquor, then through drying, broken, obtains NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer.Phosphorus potassium associated minerals are applied to prepare nitrogen-phosphorus-potassium compound fertilizer by the present invention, and the recycling of phosphorus potassium associated minerals can be achieved, and alleviate China's potash fertilizer imbalance between supply and demand；The simple production process being related to, reaction temperature is low, and can make full use of existing phosphate fertilizer manufacture craft, and equipment investment is few, energy-conserving and environment-protective.
Description
Technical field
The invention belongs to resource reutilization field, and in particular to a kind of utilization phosphorus potassium associated minerals production nitrogen-phosphorus-potassium compound fertilizer
Method.
Background technology
China's Fertilizer nutrient element ratio imbalance seriously lacks phosphorus, potassium, and urgent need greatly develops phosphorus potash fertilizer.China's phosphorus ore is generally
In, low-grade ore and mineral intergrowth, potassium ore deposit exists only in a limited number of region, and reserves are limited, and development phosphorus potash fertilizer is by multi-party
Limitation.
In recent years, the phosphorus potassium associated minerals that mound area finds collophane and potassium feldspar association are razed in Yichang City, Hubei Province, mainly into
Part is collophane and potassium feldspar, and the mineralogical composition of ore is Phosphate minerals, potassium mineral and the part of impurity three, and Phosphate minerals are mainly glue phosphorus
Ore deposit is entrained with a small amount of carbonatoapatite, francolite, in grey black；Potassium mineral is mainly slightly-inclined potassium feldspar and a small amount of orthoclase,
Impurity is mainly that muscovite, quartz and a small amount of chlorite, pyrite, limonite, ore bed thickness are 6~11m, containing P2O56~12%,
Containing K2O5~9%, generaI investigation reserves reach 800,000,000 tons.
Phosphorus, potassium grade are relatively low in phosphorus potassium associated minerals, relatively low individually with economic value, it is necessary to by beneficiation enrichment removal of impurities etc.
It can be just used effectively after industrial treatment.At this stage, phosphorus ore is generally enriched with by people by ripe ore-dressing technique, applied to phosphorus
The fields such as chemical industry, and the potassium resource in phosphorus potassium associated minerals then backfills tunnel in the form of mine tailing, causes the great wasting of resources.
The content of the invention
It is an object of the invention to provide a kind of method that utilization phosphorus potassium associated minerals produce nitrogen-phosphorus-potassium compound fertilizer, this method will
Phosphorus potassium associated minerals are applied to prepare nitrogen-phosphorus-potassium compound fertilizer, and the preparation technology being related to is simple, reaction temperature is low, energy-conserving and environment-protective.
To achieve the above object, the technical solution adopted by the present invention is：One kind utilizes phosphorus potassium associated minerals production azophoska
The method in Hefei, comprises the following steps：
1) phosphorus potassium associated minerals are carried out being crushed to≤200 mesh, then adds sulfuric acid solution, fluoride auxiliary agent, be placed in reaction
In kettle, airtight heating is to 120~150 DEG C, 1.5~2h of isothermal reaction under the conditions of pressure is carried；
2) it is that 0.03~0.1MPa, temperature are under conditions of 120~150 DEG C, to continue 0.8~2h of isothermal reaction in negative pressure
(negative reaction), obtains bottom mixture A and gas B, and the gas B ammonia absorptions obtain absorbing liquid C；
3) by step 2) gained bottom mixture A filtered, obtain filtrate D and filter residue E；Ammoniacal liquor is added into filtrate D, is adjusted
PH value is saved to 6.5~8.0, high-concentration compound N-P-K fertilizer is then evaporated, crystallizes, granulating and to obtain；Filter residue E is mixed with ammoniacal liquor
Close, then regulation pH value is dried, crushes, obtain NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer to 6.5~8.0.
In such scheme, the phosphorus potassium associated minerals contain P2O5、K2O compositions, its weight/mass percentage composition is respectively P2O510~
28%th, K2O33~11%.
In such scheme, the fluoride auxiliary agent is ammonium fluoride.
In such scheme, H in the phosphorus potassium associated minerals, sulfuric acid solution2SO4Mass ratio with ammonium fluoride is 1:(5~10):
(0.2~1.0).
In such scheme, by step 2) ammoniacal liquor is added in gained absorbing liquid C adjusts pH value to 8.5~9.5, generate titanium dioxide
Silicon is precipitated, and is no longer produced after precipitation, is filtered, obtain filtrate F and filter residue G, and filtrate F is carried out to different degrees of concentration, obtained
Ammonium fluoride phegma, fluorination ammonium concentration is 20~30wt%.
In such scheme, the ammonium fluoride phegma can be used as fluoride auxiliary agent, applied to follow-up nitrogen-phosphorus-potassium compound fertilizer
Prepare.
In such scheme, filter residue G is washed, dried, crushing to obtain white carbon.
In such scheme, the sulfuric acid solution concentration can be 60~98wt%.
The present invention reaction principle be：Phosphorus ore, cosolvent NH first in sulfuric acid and phosphorus potassium associated minerals4Companion in F and phosphorus ore
Raw fluoride reaction produces HF, and HF decomposes destruction potassium feldspar structure, and makes Mg on this basis2+、Ca2+With the K in potassium feldspar+
Generation displacement is reacted to balancing charge ion；Simultaneously by produced SiF4Gas is taken away in the form of negative pressure, it is ensured that reaction
Persistently carried out to positive direction, and reduce K2SiF6Etc. the generation of insoluble fluosilicate, improve has in gained nitrogen-phosphorus-potassium compound fertilizer
Imitate the content of nutrient.
Compared with prior art, beneficial effects of the present invention are：
1) phosphorus potassium associated minerals are applied to prepare nitrogen-phosphorus-potassium compound fertilizer by the present invention, and the recycling profit of phosphorus potassium associated minerals can be achieved
With the potash fertilizer imbalance between supply and demand of alleviation China.
2) present invention is using fluoride as auxiliary agent, and the reaction temperature being related to is low；The Ca of association in phosphorus ore can be made full use of5
(PO4)3The fluorides such as F, promote phosphorus potassium associated minerals to decompose and the nitrogen-phosphorus-potassium compound fertilizer are made；Ammonium fluoride phegma can realize fluorination
The recycling of thing auxiliary agent, energy-conserving and environment-protective.
3) present invention prepares the nitrogen-phosphorus-potassium compound fertilizer using two-step reaction, and described negative reaction can be by the SiF of generation4
Gas is taken away in the form of negative pressure, while ensuring that reaction continues to carry out to positive direction, reduces K2SiF6Etc. insoluble fluosilicic acid
The generation of salt, improves the content of available nutrient in gained nitrogen-phosphorus-potassium compound fertilizer.
4) high-concentration compound N-P-K fertilizer market conditions produced by the present invention are good, and nitrogen, phosphorus, potassium available nutrient content >=
45%；Si and Al salt in NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer exists with porous form, can play a part of water conservation, improved soil,
And with certain slow releasing function.
Brief description of the drawings
The invention will be further described below in conjunction with the accompanying drawings, in accompanying drawing：
Fig. 1 produces the process chart of nitrogen-phosphorus-potassium compound fertilizer for the present invention using phosphorus potassium associated minerals.
Embodiment
In order to be better understood from the present invention, with reference to embodiment and the accompanying drawing content that the present invention is furture elucidated, but this
The content of invention is not limited solely to the following examples.
In following examples, the phosphorus potassium associated minerals contain P2O5、K2O compositions, its weight/mass percentage composition is respectively P2O510
~28%, K2O33~11%；The fluoride auxiliary agent is ammonium fluoride chemical reagent or ammonium fluoride phegma, ammonium fluoride chemical reagent
Purity be 96wt%；Sulfuric acid solution concentration is that (density is 1.611g/cm to 70wt%3)；Ammonia concn >=25wt%.
In following examples, with reference to GB/T8572-2001《Determination of total nitrogen in compound fertilizer determines titration after distillation》、
GB/T8573-1999《Available phosphorus content is determined in Chemical Mixed Fertilizer》、GB/T8574-1988《Potassium content determines four benzene in complex fertilizer
Base closes potassium borate gravimetric method method》Etc. the content that method determines corresponding nutrient in gained nitrogen-phosphorus-potassium compound fertilizer.
Embodiment 1
A kind of method that utilization phosphorus potassium associated minerals produce nitrogen-phosphorus-potassium compound fertilizer, its technological process are as shown in figure 1, specific prepare
Method comprises the following steps：
1) phosphorus potassium associated minerals are crushed, weighs 100g phosphorus potassium associated minerals (granularity -0.074mm, 89.6%；P2O5Content
For 28wt%；K2O content is 3.9wt%), add water moistening, adds sulfuric acid solution (70wt%) 886ml and ammonium fluoride 100g, mixes
Merging is placed in reactor, and airtight heating is to 120 DEG C, the isothermal reaction 2.0h under the conditions of pressure is carried.
2) 120 DEG C are maintained, under conditions of negative pressure is 0.1MPa, continues isothermal reaction 0.8h, obtains bottoms A, negative pressure
Under the conditions of obtained gas SiF4With ammonia absorption, (NH is obtained4)2SiF6Absorbing liquid C.
3) by step 2) gained bottom mixture A filtered, obtain filtrate D and filter residue E；Filter residue E ammonifications water is adjusted into pH
To 6.5~8.0, then it is dried, crushes, obtains low concentration N P and K composite basal fertilizer；Into filtrate D ammonification water adjust pH to
6.5~8.0, then it is evaporated, crystallizes, granulates, obtains high-concentration compound N-P-K fertilizer.
4) by step 2) gained (NH4)2SiF6Absorbing liquid C adds ammoniacal liquor regulation pH to 8.5~9.5, and generation silica sinks
Form sediment and ammonium fluoride aqueous solution, no longer produce after precipitation, filtered, concentrated, obtain ammonium fluoride phegma；Precipitation of silica is done
It is dry, broken to obtain white carbon.
After testing：High-concentration compound N-P-K fertilizer total nutrient (N+P made from the present embodiment2O5+K2O content) is
45.3%, water-soluble phosphorus occupies effect phosphorus ratio 62.1%, meets standard GB/T 15063-2001《Complex fertilizer (composite fertilizer
Material)》- high concentration fertilizer index-requirement.
Si and Al salt in NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer made from the present embodiment exists with porous form, can play guarantor
The effect of water, improved soil, and with certain slow releasing function.
The present embodiment step 4) in, it is 20 that ammonium concentration is fluorinated by different concentrating degrees, in obtained ammonium fluoride phegma
~30wt%, is recycled the preparation applied to follow-up nitrogen-phosphorus-potassium compound fertilizer.
Embodiment 2
A kind of method that utilization phosphorus potassium associated minerals produce nitrogen-phosphorus-potassium compound fertilizer, the ammonium fluoride obtained using embodiment 1 is flowed back
Liquid (NH4F concentration is 27.3wt%, and density is 1.082g/cm3) as fluoride auxiliary agent, specific preparation method includes following step
Suddenly：
Weigh 100g phosphorus potassium associated minerals (granularity -0.074mm, 92.4%；P2O5Content is 10.6wt%；K2O content is
11.0wt%), 185ml ammonium fluoride phegmas are added, sulfuric acid solution (70wt%) 445ml are added after being well mixed, from pressure
With 150 DEG C under the conditions of isothermal reaction 1.5h；Then it is 0.1MPa in negative pressure and temperature is under conditions of 150 DEG C, to continue constant temperature anti-
0.8h is answered, other step be the same as Examples 1.
After testing：High-concentration compound N-P-K fertilizer total nutrient (N+P made from the present embodiment2O5+K2O content) is
37.6%, water-soluble phosphorus occupies effect phosphorus ratio 52.7%, meets standard GB/T 15063-2001《Complex fertilizer (composite fertilizer
Material)》The requirement of-middle analysis fertilizer index-.
Embodiment 3
A kind of method that utilization phosphorus potassium associated minerals produce nitrogen-phosphorus-potassium compound fertilizer, the ammonium fluoride obtained using embodiment 1 is flowed back
Liquid (NH4F concentration is 20.4wt%, and density is 1.070g/cm3) as fluoride auxiliary agent, specific preparation method includes following step
Suddenly：
Weigh 100g phosphorus potassium associated minerals (granularity -0.074mm, 88.7%；P2O5Content is 22.7wt%, K2O content is
6wt%), 120ml ammonium fluoride phegmas are added, sulfuric acid solution (70wt%) 798ml is added after being well mixed, in self-generated pressure and
Isothermal reaction 1.5h under the conditions of 140 DEG C；It is again 0.04MPa in negative pressure and temperature is under conditions of 140 DEG C, to continue isothermal reaction
1.0h, other step be the same as Examples 1.
After testing：High-concentration compound N-P-K fertilizer total nutrient (N+P made from the present embodiment2O5+K2O content) is
47.8%, water-soluble phosphorus occupies effect phosphorus ratio 65.7%, meets standard GB/T 15063-2001《Complex fertilizer (composite fertilizer
Material)》- high concentration fertilizer index-requirement.
Comparative example
Take three groups of raw materials, I groups：Phosphorus potassium associated minerals 1g, sulfuric acid solution (70wt%) 6.7g；II groups and III groups：Phosphorus potassium association
Ore deposit 1g, sulfuric acid solution (70wt%) 6.7g, 0.5g ammonium fluoride.Specific preparation process is as follows：I group raw materials are sufficiently mixed, in 120
DEG C isothermal reaction 3h；II group raw materials are sufficiently mixed, in 120 DEG C of constant temperature 3h；III group raw materials are sufficiently mixed, in 120 DEG C of constant temperature 2.2h
Afterwards, then under conditions of negative pressure is 0.1MPa, in reacting 0.8h at 120 DEG C.
Solubility K in three groups of raw material reaction products is measured respectively+Dissolution rate and solubility PO4 3-Dissolution rate, as a result see
Table 1.
Table 1
As can be seen from Table 1, in the reaction product of three groups of raw materials, phosphate anion dissolution rate is substantially suitable, but potassium ion
Dissolution rate difference is very big.Illustrate to add sulfuric acid and ammonium fluoride in phosphorus potassium associated minerals, can be under cryogenic, it is ensured that phosphate is higher
Dissolution rate, and improve the dissolution rate of potassium, effectively reduce energy consumption, material consumption；And negative reaction process can further improve the molten of potassium
Extracting rate, is conducive to the preparation of nitrogen-phosphorus-potassium compound fertilizer.
It the foregoing is only the preferred embodiment of the present invention, it is noted that come for one of ordinary skill in the art
Say, without departing from the concept of the premise of the invention, make some modifications and variations, these belong to the protection model of the present invention
Enclose.
Claims (7)
1. the method for nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals, it is characterised in that comprise the following steps：
1) phosphorus potassium associated minerals are crushed, then adds sulfuric acid, fluoride auxiliary agent, be placed in reactor, airtight heating to 120
~150 DEG C, 1.5~2h of isothermal reaction under the conditions of pressure is carried；
2) it is that 0.03~0.1MPa, temperature are under conditions of 120~150 DEG C, to continue 0.8~2h of isothermal reaction, obtain kettle in negative pressure
Bottom mixture A and gas B, the gas B ammonia absorptions, obtain absorbing liquid C；
3) by step 2) gained bottom mixture A filtered, obtain filtrate D and filter residue E；Ammoniacal liquor is added into filtrate D, is adjusted
Then pH value is evaporated, crystallizes, granulating and to obtain high-concentration compound N-P-K fertilizer to 6.5~8.0；Filter residue E is mixed with ammoniacal liquor,
PH value is adjusted to 6.5~8.0, is then dried, crushes, obtain NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer；
The fluoride auxiliary agent is ammonium fluoride.
2. the method for nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals according to claim 1, it is characterised in that the phosphorus
Potassium associated minerals contain P2O5、K2O compositions, its weight/mass percentage composition is respectively P2O510~28%, K2O33~11%.
3. the method for nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals according to claim 1, it is characterised in that the phosphorus
H in potassium associated minerals, sulfuric acid2SO4Mass ratio with ammonium fluoride is 1:(5~10):(0.2~1.0).
4. the method for producing nitrogen-phosphorus-potassium compound fertilizer according to any one of claims 1 to 3 utilization phosphorus potassium associated minerals, its feature exists
In by step 2) add ammoniacal liquor in gained absorbing liquid C and adjust pH value to 8.5~9.5, generate precipitation of silica, when precipitation not
When being further added by, filtered, obtain filtrate F and filter residue G, filtrate F is concentrated, obtain ammonium fluoride phegma, be fluorinated ammonium concentration
For 20~30wt%.
5. the method for nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals according to claim 4, it is characterised in that the fluorine
Change ammonium phegma and be used as fluoride auxiliary agent.
6. the method for nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals according to claim 4, it is characterised in that by filter residue
G is washed, dried, crushing to obtain white carbon.
7. the method for nitrogen-phosphorus-potassium compound fertilizer is produced using phosphorus potassium associated minerals according to claim 4, it is characterised in that the phosphorus
Potassium associated minerals are crushed to≤200 mesh.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367176B (en) * | 2015-12-02 | 2019-03-08 | 武汉工程大学 | A kind of multielement composite of phosphorus potassium associated minerals utilizes technique |
| CN105603215B (en) * | 2015-12-30 | 2017-12-19 | 武汉工程大学 | One kind efficiently leaches K, Ca, Mg, P method using extractant and hydrochloric acidolysis technology from phosphorus potassium associated minerals |
| 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 |
| 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 |
| 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 |
| CN113173584A (en) * | 2021-04-21 | 2021-07-27 | 武汉工程大学 | Resource comprehensive utilization method of phosphorus tailings and potassium feldspar |
| CN115535976B (en) * | 2022-10-13 | 2024-02-23 | 中国科学院过程工程研究所 | Device system and method for recycling potassium-containing phosphorite |
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| US4191734A (en) * | 1976-06-15 | 1980-03-04 | Pennzoil Company | Fluoride-free phosphate reactions |
| CN86106384A (en) * | 1986-09-23 | 1987-04-22 | 路文兴 | The direct extraction method of phosphoric acid of high ferro aluminium phosphorus ore |
| CN1083034A (en) * | 1992-07-13 | 1994-03-02 | 成都科技大学 | The production method of ammonium potassium dihydrogen phosphate |
| CN101633584A (en) * | 2009-08-07 | 2010-01-27 | 山东科技大学 | A method for producing nitrogen phosphorus potassium compound fertilizer with water-insoluble potassium-containing rock |
| CN101704687A (en) * | 2009-09-28 | 2010-05-12 | 陈锋 | Method for producing potassium sulphate by decomposing potassium feldspar at low temperature |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4191734A (en) * | 1976-06-15 | 1980-03-04 | Pennzoil Company | Fluoride-free phosphate reactions |
| CN86106384A (en) * | 1986-09-23 | 1987-04-22 | 路文兴 | The direct extraction method of phosphoric acid of high ferro aluminium phosphorus ore |
| CN1083034A (en) * | 1992-07-13 | 1994-03-02 | 成都科技大学 | The production method of ammonium potassium dihydrogen phosphate |
| CN101633584A (en) * | 2009-08-07 | 2010-01-27 | 山东科技大学 | A method for producing nitrogen phosphorus potassium compound fertilizer with water-insoluble potassium-containing rock |
| CN101704687A (en) * | 2009-09-28 | 2010-05-12 | 陈锋 | Method for producing potassium sulphate by decomposing potassium feldspar at low temperature |
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