CN104744175A - Method for producing nitrogen-phosphorus-potassium mixed fertilizer by utilizing phosphorus-potassium associated ore - Google Patents
Method for producing nitrogen-phosphorus-potassium mixed fertilizer by utilizing phosphorus-potassium associated ore Download PDFInfo
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Abstract
The invention discloses a method for producing a nitrogen-phosphorus-potassium mixed fertilizer by utilizing phosphorus-potassium associated ore. The method comprises the following steps: by taking the phosphorus-potassium associated ore as a raw material, mixing with sulfuric acid and fluoride aids in a reaction kettle, heating, sequentially reacting in the reactor under the reactor pressure and negative pressure conditions, filtering the kettle substrate after the reaction is ended, regulating the pH value of the obtained filtrate to be 6.5-8.0 by using ammonia water, evaporating, crystallizing, and granulating, thereby obtaining a high-concentration nitrogen-phosphorus-potassium mixed fertilizer; and regulating the pH value of the obtained filter residues to be 6.5-8.0 by using ammonia water, drying, and crushing, thereby obtaining the low-concentration nitrogen-phosphorus-potassium mixed fertilizer. According to the method disclosed by the invention, the phosphorus-potassium associated ore is applied to preparing the nitrogen-phosphorus-potassium mixed fertilizer, the phosphorus-potassium associated ore can be recycled, and the imbalance between supply and demand of the potash fertilizers in China is relieved; and moreover, the involved production process is simple, the reaction temperature is low, the conventional potash fertilizer preparation process can be fully utilized, the equipment investment is low, and the method is energy-saving and environment-friendly.
Description
Technical field
The invention belongs to resource reutilization field, be specifically related to a kind of method utilizing phosphorus potassium associated minerals to produce nitrogen-phosphorus-potassium compound fertilizer.
Background technology
China's Fertilizer nutrient element ratio imbalance is serious lacks phosphorus, potassium, is badly in need of greatly developing phosphorus potash fertilizer.During China's phosphorus ore mostly is, low grade ore and mineral intergrowth, potassium ore deposit is only present in limited several regions, and reserves are limited, and development phosphorus potash fertilizer is limited in many ways.
In recent years, area, smooth mound, Yichang City, Hubei Province finds the phosphorus potassium associated minerals of collophanite and potassium felspar sand association, major ingredient is collophanite and potassium felspar sand, the mineralogical composition of ore is Phosphate minerals, potassium mineral and impurity three part, Phosphate minerals is mainly collophanite and is entrained with a small amount of podolite, francolite, in grey black; Potassium mineral is mainly slightly-inclined potassium felspar sand and a small amount of potash feldspar, and impurity is mainly white mica, quartz and a small amount of chlorite, pyrite, limonite, ore bed is thick is 6 ~ 11m, containing P
2o
56 ~ 12%, containing K
2o5 ~ 9%, generaI investigation reserves reach 800,000,000 tons.
Phosphorus in phosphorus potassium associated minerals, potassium grade are lower, utilize separately economic worth lower, just can be used effectively after having to pass through the industrial treatment such as beneficiation enrichment removal of impurities.Present stage, people pass through ripe ore-dressing technique usually by phosphorus ore enrichment, are applied to the fields such as phosphorous chemical industry, and the potassium resource in phosphorus potassium associated minerals then with the form of mine tailing backfill tunnel, causes the great wasting of resources.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing phosphorus potassium associated minerals to produce nitrogen-phosphorus-potassium compound fertilizer, phosphorus potassium associated minerals are applied to by the method prepares nitrogen-phosphorus-potassium compound fertilizer, and the preparation technology related to is simple, temperature of reaction is low, energy-conserving and environment-protective.
For achieving the above object, the technical solution used in the present invention is: a kind of method utilizing phosphorus potassium associated minerals to produce nitrogen-phosphorus-potassium compound fertilizer, comprises the following steps:
1) phosphorus potassium associated minerals are carried out being crushed to≤200 orders, then add sulphuric acid soln, fluorochemical auxiliary agent, be placed in reactor, be airtightly heated to 120 ~ 150 DEG C, carrying isothermal reaction 1.5 ~ 2h under press strip part;
2) negative pressure be 0.03 ~ 0.1MPa, under temperature is the condition of 120 ~ 150 DEG C, continue isothermal reaction 0.8 ~ 2h (negative reaction), obtain mixture A at the bottom of still and gas B, described gas B ammonia absorption, obtains absorption liquid C;
3) by step 2) mixture A at the bottom of gained still filters, and obtains filtrate D and filter residue E; In filtrate D, add ammoniacal liquor, adjust ph to 6.5 ~ 8.0, then carry out evaporating, crystallization, granulation obtain high-concentration compound N-P-K fertilizer; Filter residue E is mixed with ammoniacal liquor, adjust ph to 6.5 ~ 8.0, then carry out drying, fragmentation, obtain NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer.
In such scheme, described phosphorus potassium associated minerals contain P
2o
5, K
2o composition, its mass percentage is respectively P
2o
510 ~ 28%, K
2o
33 ~ 11%.
In such scheme, described fluorochemical auxiliary agent is Neutral ammonium fluoride.
In such scheme, H in described phosphorus potassium associated minerals, sulphuric acid soln
2sO
4be 1:(5 ~ 10 with the mass ratio of Neutral ammonium fluoride): (0.2 ~ 1.0).
In such scheme, by step 2) add ammoniacal liquor adjust ph to 8.5 ~ 9.5 in gained absorption liquid C, generate precipitation of silica, after no longer producing precipitation, filter, obtain filtrate F and filter residue G, that is carried out by filtrate F in various degree is concentrated, obtain Neutral ammonium fluoride phegma, Neutral ammonium fluoride concentration is 20 ~ 30wt%.
In such scheme, described Neutral ammonium fluoride phegma can be used as fluorochemical auxiliary agent, is applied to the preparation of follow-up nitrogen-phosphorus-potassium compound fertilizer.
In such scheme, filter residue G is carried out wash, dry, broken white carbon black.
In such scheme, described sulphuric acid soln concentration can be 60 ~ 98wt%.
Reaction principle of the present invention is: phosphorus ore, solubility promoter NH first in sulfuric acid and phosphorus potassium associated minerals
4the fluorochemical reaction of association in F and phosphorus ore produces HF, HF and decomposes and destroy potassium felspar sand structure, and makes Mg on this basis
2+, Ca
2+with the K in potassium felspar sand
+there is replacement(metathesis)reaction and become balancing charge ion; Simultaneously by produced SiF
4gas is taken away with the form of negative pressure, guarantees that reaction continues to carry out to positive dirction, and reduces K
2siF
6etc. the generation of insoluble silicofluoride, improve the content of available nutrient in gained nitrogen-phosphorus-potassium compound fertilizer.
Compared with prior art, beneficial effect of the present invention is:
1) phosphorus potassium associated minerals are applied to and prepare nitrogen-phosphorus-potassium compound fertilizer by the present invention, can realize the recycling of phosphorus potassium associated minerals, alleviate China's potash fertilizer imbalance between supply and demand.
2) the present invention adopts fluorochemical as auxiliary agent, and the temperature of reaction related to is low; The Ca of association in phosphorus ore can be made full use of
5(PO
4)
3the fluorochemicals such as F, promote that phosphorus potassium associated minerals decompose obtained described nitrogen-phosphorus-potassium compound fertilizer; Neutral ammonium fluoride phegma can realize the recycling of fluorochemical auxiliary agent, energy-conserving and environment-protective.
3) the present invention adopts two-step reaction to prepare described nitrogen-phosphorus-potassium compound fertilizer, the SiF that described negative reaction can will produce
4gas is taken away with the form of negative pressure, while guaranteeing to react and continuing to carry out to positive dirction, reduces K
2siF
6etc. the generation of insoluble silicofluoride, improve the content of available nutrient in gained nitrogen-phosphorus-potassium compound fertilizer.
4) the high-concentration compound N-P-K fertilizer market conditions that obtain of the present invention are good, 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 the effect of water conservation, improvement soil, and have certain slow releasing function.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described, in accompanying drawing:
Fig. 1 is that the present invention utilizes phosphorus potassium associated minerals to produce the process flow sheet of nitrogen-phosphorus-potassium compound fertilizer.
Embodiment
For a better understanding of the present invention, illustrate content of the present invention further below in conjunction with embodiment and accompanying drawing, but content of the present invention is not only confined to the following examples.
In following examples, described phosphorus potassium associated minerals contain P
2o
5, K
2o composition, its mass percentage is respectively P
2o
510 ~ 28%, K
2o
33 ~ 11%; Described fluorochemical auxiliary agent is Neutral ammonium fluoride chemical reagent or Neutral ammonium fluoride phegma, and the purity of Neutral ammonium fluoride chemical reagent is 96wt%; Sulphuric acid soln concentration is that (density is 1.611g/cm to 70wt%
3); Ammonia concn>=25wt%.
In following examples, measure the content of corresponding nutrient in gained nitrogen-phosphorus-potassium compound fertilizer with reference to methods such as GB/T8572-2001 " determination of total nitrogen in compound fertilizer measures the rear volumetry of distillation ", GB/T8573-1999 " in Chemical Mixed Fertilizer, available phosphorus content measures ", GB/T8574-1988 " in composite fertilizer, potassium content measures tetraphenyl and closes potassium borate weighting method method ".
Embodiment 1
Utilize phosphorus potassium associated minerals to produce a method for nitrogen-phosphorus-potassium compound fertilizer, as shown in Figure 1, concrete preparation method comprises the following steps in its technical process:
1) phosphorus potassium associated minerals are carried out fragmentation, take 100g phosphorus potassium associated minerals (granularity-0.074mm, 89.6%; P
2o
5content is 28wt%; K
2o content is 3.9wt%), add water moistening, add sulphuric acid soln (70wt%) 886ml and Neutral ammonium fluoride 100g, mix and be placed in reactor, be airtightly heated to 120 DEG C, carrying isothermal reaction 2.0h under press strip part.
2) maintaining 120 DEG C, is under the condition of 0.1MPa in negative pressure, continues isothermal reaction 0.8h, obtains bottoms A, the gas SiF obtained under condition of negative pressure
4with ammonia absorption, obtain (NH
4)
2siF
6absorption liquid C.
3) by step 2) mixture A at the bottom of gained still filters, and obtains filtrate D and filter residue E; Filter residue E is added ammoniacal liquor and regulate pH to 6.5 ~ 8.0, then carry out drying, fragmentation, obtain lower concentration N P and K composite basal fertilizer; In filtrate D, add ammoniacal liquor regulate pH to 6.5 ~ 8.0, then carry out evaporating, crystallization, granulation, obtain high-concentration compound N-P-K fertilizer.
4) by step 2) gained (NH
4)
2siF
6absorption liquid C adds ammoniacal liquor and regulates pH to 8.5 ~ 9.5, generates precipitation of silica and ammonium fluoride aqueous solution, after no longer producing precipitation, carries out filtering, concentrating, obtains Neutral ammonium fluoride phegma; White carbon black is obtained by dry, broken for precipitation of silica.
After testing: the high-concentration compound N-P-K fertilizer total nutrient (N+P that the present embodiment is obtained
2o
5+ K
2o) content is 45.3%, water-soluble phosphorus occupy effect phosphorus ratio 62.1%, meet standard GB/T 15063-2001 " composite fertilizer (compound manure) "-high concentration fertilizer index-requirement.
Si and Al salt in the NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer that the present embodiment obtains exists with porous form, can play the effect of water conservation, improvement soil, and have certain slow releasing function.
The present embodiment step 4) in, by different concentrating degree, in the Neutral ammonium fluoride phegma obtained, Neutral ammonium fluoride concentration is 20 ~ 30wt%, the preparation being applied to follow-up nitrogen-phosphorus-potassium compound fertilizer capable of circulation.
Embodiment 2
Utilize phosphorus potassium associated minerals to produce a method for nitrogen-phosphorus-potassium compound fertilizer, adopt the Neutral ammonium fluoride phegma (NH that embodiment 1 obtains
4f concentration is 27.3wt%, and density is 1.082g/cm
3) as fluorochemical auxiliary agent, concrete preparation method comprises the following steps:
Take 100g phosphorus potassium associated minerals (granularity-0.074mm, 92.4%; P
2o
5content is 10.6wt%; K
2o content is 11.0wt%), add 185ml Neutral ammonium fluoride phegma, after mixing, add sulphuric acid soln (70wt%) 445ml, at isothermal reaction 1.5h under with pressure and 150 DEG C of conditions; Then, under be 0.1MPa and temperature being the condition of 150 DEG C in negative pressure, continue isothermal reaction 0.8h, other steps are with embodiment 1.
After testing: the high-concentration compound N-P-K fertilizer total nutrient (N+P that the present embodiment is obtained
2o
5+ K
2o) content is 37.6%, water-soluble phosphorus occupy effect phosphorus ratio 52.7%, meet standard GB/T 15063-2001 " composite fertilizer (compound manure) "-middle analysis fertilizer index-requirement.
Embodiment 3
Utilize phosphorus potassium associated minerals to produce a method for nitrogen-phosphorus-potassium compound fertilizer, adopt the Neutral ammonium fluoride phegma (NH that embodiment 1 obtains
4f concentration is 20.4wt%, and density is 1.070g/cm
3) as fluorochemical auxiliary agent, concrete preparation method comprises the following steps:
Take 100g phosphorus potassium associated minerals (granularity-0.074mm, 88.7%; P
2o
5content is 22.7wt%, K
2o content is 6wt%), add 120ml Neutral ammonium fluoride phegma, after mixing, add sulphuric acid soln (70wt%) 798ml, isothermal reaction 1.5h under autogenous pressure and 140 DEG C of conditions; Under be 0.04MPa and temperature being the condition of 140 DEG C in negative pressure again, continue isothermal reaction 1.0h, other steps are with embodiment 1.
After testing: the high-concentration compound N-P-K fertilizer total nutrient (N+P that the present embodiment is obtained
2o
5+ K
2o) content is 47.8%, water-soluble phosphorus occupy effect phosphorus ratio 65.7%, meet standard GB/T 15063-2001 " composite fertilizer (compound manure) "-high concentration fertilizer index-requirement.
Comparative example
Get three groups of raw materials, I group: phosphorus potassium associated minerals 1g, sulphuric acid soln (70wt%) 6.7g; II group and III group: phosphorus potassium associated minerals 1g, sulphuric acid soln (70wt%) 6.7g, 0.5g Neutral ammonium fluoride.Concrete preparation process is as follows: fully mixed by I group raw material, in 120 DEG C of isothermal reaction 3h; II group raw material fully mixes, in 120 DEG C of constant temperature 3h; III group raw material fully mixes, after 120 DEG C of constant temperature 2.2h, then in negative pressure be 0.1MPa condition under, at 120 DEG C, react 0.8h.
Measure solubility K in three groups of raw material reaction products respectively
+solubility rate and solubility PO
4 3-solubility rate, the results are shown in Table 1.
Table 1
As can be seen from Table 1, in the reaction product of three groups of raw materials, phosphate anion solubility rate is substantially suitable, but the difference of potassium ion solubility rate greatly.Illustrate and add sulfuric acid and Neutral ammonium fluoride at phosphorus potassium associated minerals, under cryogenic, the solubility rate that phosphoric acid salt is higher can be guaranteed, and improve the solubility rate of potassium, effectively reduce energy consumption, material consumption; And negative reaction process can further improve the solubility rate of potassium, be conducive to the preparation of nitrogen-phosphorus-potassium compound fertilizer.
The foregoing is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, without departing from the concept of the premise of the invention, make some improvement and conversion, these all belong to protection scope of the present invention.
Claims (8)
1. utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer, it is characterized in that, comprise the following steps:
1) phosphorus potassium associated minerals are carried out fragmentation, then add sulfuric acid, fluorochemical auxiliary agent, be placed in reactor, be airtightly heated to 120 ~ 150 DEG C, carry isothermal reaction 1.5 ~ 2h under press strip part;
2) negative pressure be 0.03 ~ 0.1MPa, under temperature is the condition of 120 ~ 150 DEG C, continue isothermal reaction 0.8 ~ 2h, obtain mixture A at the bottom of still and gas B, described gas B ammonia absorption, obtains absorption liquid C;
3) by step 2) mixture A at the bottom of gained still filters, and obtains filtrate D and filter residue E; In filtrate D, add ammoniacal liquor, adjust ph to 6.5 ~ 8.0, then carry out evaporating, crystallization, granulation obtain high-concentration compound N-P-K fertilizer; Filter residue E is mixed with ammoniacal liquor, adjust ph to 6.5 ~ 8.0, then carry out drying, fragmentation, obtain NITROGEN IN LOW CONCENTRATION phosphorus potassium complex fertilizer.
2. utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer according to claim 1, it is characterized in that, described phosphorus potassium associated minerals contain P
2o
5, K
2o composition, its mass percentage is respectively P
2o
510 ~ 28%, K
2o
33 ~ 11%.
3. utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer according to claim 1, it is characterized in that, described fluorochemical auxiliary agent is Neutral ammonium fluoride.
4. utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer according to claim 3, it is characterized in that, H in described phosphorus potassium associated minerals, sulfuric acid
2sO
4be 1:(5 ~ 10 with the mass ratio of Neutral ammonium fluoride): (0.2 ~ 1.0).
5. according to any one of Claims 1 to 4, utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer, it is characterized in that, by step 2) add ammoniacal liquor adjust ph to 8.5 ~ 9.5 in gained absorption liquid C, generate precipitation of silica, when precipitation no longer increases, filter, obtain filtrate F and filter residue G, concentrated by filtrate F, obtain Neutral ammonium fluoride phegma, Neutral ammonium fluoride concentration is 20 ~ 30wt%.
6. utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer according to claim 5, it is characterized in that, described Neutral ammonium fluoride phegma is used as fluorochemical auxiliary agent.
7. utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer according to claim 5, it is characterized in that, filter residue G is carried out wash, dry, broken white carbon black.
8. utilize phosphorus potassium associated minerals to produce the method for nitrogen-phosphorus-potassium compound fertilizer according to claim 1, it is characterized in that, described phosphorus potassium associated minerals are crushed to≤200 orders.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367176A (en) * | 2015-12-02 | 2016-03-02 | 武汉工程大学 | Multi-element comprehensive utilization process for phosphorus-potassium associated ore |
| CN105603215A (en) * | 2015-12-30 | 2016-05-25 | 武汉工程大学 | Method using extraction agent and hydrochloric acid acidolysis technology to efficiently leach K, Ca, Mg and P from P and K associated 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 |
| CN112758937A (en) * | 2021-01-14 | 2021-05-07 | 襄阳泽东化工集团有限公司 | Method for preparing potassium fluosilicate and NPK compound fertilizer from phosphorus-potassium associated ore |
| CN112898073A (en) * | 2021-01-14 | 2021-06-04 | 襄阳泽东化工集团有限公司 | Method for preparing NPK compound fertilizer by using phosphate tailings 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 |
| CN115535976A (en) * | 2022-10-13 | 2022-12-30 | 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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367176A (en) * | 2015-12-02 | 2016-03-02 | 武汉工程大学 | Multi-element comprehensive utilization process for phosphorus-potassium associated ore |
| 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 |
| CN105603215A (en) * | 2015-12-30 | 2016-05-25 | 武汉工程大学 | Method using extraction agent and hydrochloric acid acidolysis technology to efficiently leach K, Ca, Mg and P from P and K associated ore |
| CN112758937A (en) * | 2021-01-14 | 2021-05-07 | 襄阳泽东化工集团有限公司 | Method for preparing potassium fluosilicate and NPK compound fertilizer from phosphorus-potassium associated ore |
| CN112898073A (en) * | 2021-01-14 | 2021-06-04 | 襄阳泽东化工集团有限公司 | 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 |
| CN113173584A (en) * | 2021-04-21 | 2021-07-27 | 武汉工程大学 | Resource comprehensive utilization method of phosphorus tailings and potassium feldspar |
| CN115535976A (en) * | 2022-10-13 | 2022-12-30 | 中国科学院过程工程研究所 | Device system and method for recycling potassium-containing phosphorite |
| 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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