CN105859329A - Method for preparing nitro phosphate containing polyphosphate and multiple nutrient elements - Google Patents
Method for preparing nitro phosphate containing polyphosphate and multiple nutrient elements Download PDFInfo
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- CN105859329A CN105859329A CN201610196551.9A CN201610196551A CN105859329A CN 105859329 A CN105859329 A CN 105859329A CN 201610196551 A CN201610196551 A CN 201610196551A CN 105859329 A CN105859329 A CN 105859329A
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- quadrafos
- pressure
- nutrient elements
- nano material
- acid
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/04—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
- C05B11/06—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using nitric acid (nitrophosphates)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Soil Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a method for preparing nitro phosphate containing a polyphosphate and multiple nutrient elements. The method comprises the steps of (1) the mixed-decomposition of apatite by using nitric acid and phosphoric acid; (2) ammonium neutralization; (3) the addition of sylvite; (4) granulation. The method also comprises the steps of reducing the pressure to be lower than 0.05 MPa, evaporating, and concentrating till the water content of a product is smaller than or equal to 2% by weight; heating till the temperature reaches over 170 DEG C, increasing the pressure till the pressure is larger than the atmospheric pressure, and subjecting the product to polymerization reaction to produce a polyphosphate; processing ore materials by using a nano grinder, wherein ore materials are composed of stone powders, diatomite, bentonite, magnesite, humic acid, and the like; subjecting the materials to wet grinding till the particle sizes of the materials are below 100 nm; granulating again to obtain the nitro phosphate containing the polyphosphate and multiple nutrient elements. According to the technical scheme of the invention, the defect in the prior art that the conventional nitro phosphate only contains single NPK components can be overcome. Nano materials containing ore materials as raw materials are added in before the granulating step. In this way, not only the nano materials serve as nutrients, but also the synergistic effect based on the nano structure is realized. At the same time, the nitro phosphate contains the polyphosphate.
Description
Technical field
The present invention relates to field of compound fertilizer production, particularly relate to a kind of nitrophosphate fertilizer containing Quadrafos and various nutrient elements
Preparation method.
Background technology
Existing nitric acid phosphoric acid process as it is shown in figure 1, the technical process of preparing nitrophosphate fertilizer is that phosphorus ore and nitric acid are added acidolysis groove,
Controlling temperature 50-65 DEG C, acid hydrolysis solution enters one section of reactive tank, adds phosphoric acid and ammonia at this, neutralizes, controls temperature 110-130 DEG C；
In second-stage reaction groove, adding potassium salt and middle trace element, direct pelletize obtains nitrophosphate fertilizer.This process is micro-in having related to
Secondary element, but the nanostructured of not mentioned material, do not evaporate before pelletizing meanwhile, concentrate, and does not contains Quadrafos.
Nano material has a series of special physics and chemical property, including small-size effect, surface-interface effect etc., absorbing,
The aspects such as catalysis, magnetic effect show special character.
CN200780044974.8 discloses a kind of nitrophosphate process and produces containing polyphosphate NPK or the method for NP material,
The method is by reducing the pressure of evaporation step and/or improving the temperature of evaporation step and/or control the temperature of crystallisation step so that
To material in containing the mixture of MAP, DAP, DCP and optional apatite, and condensed phosphate (many phosphorus of controlled quentity controlled variable
Hydrochlorate), and N/P and Ca/P of NPK material is than for N/P >=0.95,1.0 >=Ca/P >=0.2, and obtained by the method
Product.The method of preparing nitrophosphate fertilizer being also disclosed simultaneously, comprises the steps of (1) nitric acid digestion apatite, (2) crystallize,
Filtration of calcium nitrate, (3) neutralize with ammonia, and (4) evaporate, and wherein the pressure of evaporation process reduction evaporation makes moisture be less than or equal to
1%, optionally improve the temperature of step (4) simultaneously, optionally control the temperature of crystallisation step (2) thus generate polyphosphate,
Optionally add potassium afterwards in step (4)；Prior art can only realize the chemical reaction of APP under negative pressure and generate, and condition limits
System is relatively stricter, and power consumption height, is unfavorable for reaching the purpose of energy-saving and emission-reduction, and this technology the most discloses nano-scale carbon, receives
The rice nutrient such as humic acid and nanoscale calcium and magnesium silicon is reasonably applied in nitrophosphate fertilizer product, ensures poly-phosphorus in product simultaneously
The degree of polymerization of acid ammonium and aggregate rate can guarantee that again various nutrient elements meets plant growth demand, calcium and magnesium silicon of the prior art unit
Element is easy to make phosphate lose efficacy with phosphate reaction.
CN104030808A discloses a kind of durable action composition and the method preparing water-soluble controlled availability fertilizer with durable action composition, this
The polyamino acid that consists of of bright durable action composition is 5-25%, and Quadrafos is 10-30%, and polyacrylate is 0.5-5%, long
Effect agent is 25-45%, and humic acid material is 5-15%, and the mass percent sum of each component is equal to 100.Although this technology
Disclosing Quadrafos and fertilizer prepared by humic acid, but do not select nano material, nanoscale structures is due to surface atom
Around lack adjacent atom, there is unsaturation, easily combine with other atoms and settle out, show the highest change
Learning activity, along with the reduction of particle diameter, the surface area of nano fertilizer particle, surface energy and Surface binding energy increase the most rapidly, hold
Easily adsorbed by plant, improve the utilization ratio of fertilizer, the most do not disclose suitable condition to prepare the Quadrafos of high polymerization degree
Nitrophosphate fertilizer with various nutrient elements.
Summary of the invention
The defect that the present invention is directed to prior art provides a kind of containing Quadrafos and the preparation side of the nitrophosphate fertilizer of various nutrient elements
Method.
The object of the invention is achieved through the following technical solutions.
A kind of containing Quadrafos and the preparation method of the nitrophosphate fertilizer of various nutrient elements, comprise the following steps:
(1) with nitric acid and phosphoric acid mixed decomposition apatite；
(2) ammonia neutralizes；
(3) potassium salt is added；
(4) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(5) temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction to generate Quadrafos；
(6) nano material is added in Quadrafos, then carry out pelletize and obtain the nitre containing Quadrafos and various nutrient elements
Acid phosphate fertilizer.
Described nano material comprises nano-sized carbon or nanometer humic acid and utilizes the mach ore materials of sand milling, such as stone powder, diatom
One or more in soil, bentonite, four kinds of ore materials of magnesite, the mean diameter of nano material is less than 100nm；
The addition of institute's nano material accounts for the 0.1%-5% of weight of fertilizer.
Or, a kind of containing Quadrafos and the preparation method of the nitrophosphate fertilizer of various nutrient elements, it is also possible to comprise the following steps:
(1) with nitric acid and phosphoric acid mixed decomposition apatite；
(2) ammonia neutralizes；
(3) potassium salt is added；
(4) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(5) adding in concentrated solution by nano material, temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction raw
Become containing Quadrafos and the nitrophosphate fertilizer of various nutrient elements.
Described nano material comprises nano-sized carbon or nanometer humic acid and utilizes the mach ore materials of sand milling, such as stone powder, diatom
One or more in soil, bentonite, four kinds of ore materials of magnesite, the mean diameter of nano material is less than 100nm；
The addition of described nano material accounts for the 0.1%-5% of weight of fertilizer.
Preferably, the particle diameter of described nano material is 50～100nm.
Above-mentioned nitric acid, phosphoric acid, apatite, the consumption of potassium salt are any proportioning, it is preferred that described nitric acid, phosphoric acid, phosphorus ash
Stone, the weight ratio of potassium salt be, nitric acid: phosphoric acid: apatite: potassium salt=1～100:1～100:1～100:1～100.
The present invention provides a kind of containing Quadrafos and the nitrophosphate fertilizer of various nutrient elements, and the preparation method of described nitrophosphate fertilizer is such as
Under:
(1) with nitric acid and phosphoric acid mixed decomposition apatite；
(2) ammonia neutralizes；
(3) potassium salt is added；
(3) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(4) temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction to generate Quadrafos；
(5) nano material is added in Quadrafos, then carry out pelletize and obtain the nitre containing Quadrafos and various nutrient elements
Acid phosphate fertilizer；
Described nano material comprises nano-sized carbon or nanometer humic acid and stone powder, kieselguhr, bentonite, four kinds of Ore materials of magnesite
One or more in material, mean diameter is less than 100nm.
The present invention provides a kind of containing Quadrafos and the nitrophosphate fertilizer of various nutrient elements, and the preparation method of described nitrophosphate fertilizer is such as
Under:
(1) with nitric acid and phosphoric acid mixed decomposition apatite；
(2) ammonia neutralizes；
(3) potassium salt is added；
(4) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(5) adding nano material, temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction to generate containing poly-phosphorus
Hydrochlorate and the nitrophosphate fertilizer of multiple nutritional components；
Described nano material comprises nano-sized carbon or nanometer humic acid and stone powder, kieselguhr, bentonite, four kinds of Ore materials of magnesite
One or more in material, mean diameter is less than 100nm.
The present invention is relative to prior art have the advantage that and beneficial effect.
(1), the problem of N P and K it is confined to for nitrophosphate fertilizer nutrient, trace element in proposing to add before pelletize, including
One or several combinations in calcium, magnesium, silicon etc.；
(2), the nano material that adds there is the function of nutrient, and form for Raw material processing with Ore, this material is
Nanoscale structures, stable chemical nature, do not react with other composition in nitrophosphate fertilizer, do not react with Quadrafos,
This point is that phosphate anion is more stable effectively；
(3) the nanoscale humic acid, in the present invention is possible not only to adsorption activation nutrient calcium, magnesium, silicon, prevents nutrition unit
Element is combined with phosphate anion, improves the effective percentage of phosphate radical, it is also possible to be combined formation phosphoric acid-phosphate with insoluble phosphate,
Phosphate is made to activate so that it is to be more easy to absorbed by crops；Nano-sized carbon or nanometer humic acid can also improve carbon source nutrition for crop；
(4), the shortcoming of the degree of polymerization of polyphosphoric acid can not be improved for this link of transpiring moisture, propose utilize normal pressure or add
The mode of pressure is distilled, and improves the degree of polymerization and aggregate rate, and APP has that chemical stability is good, hygroscopicity is little, dispersibility is excellent
Good, proportion is little, low toxin；
(5) Quadrafos of high polymerization degree combines mineral element and is more easy to be adsorbed by root system under the effect of nanoscale humic acid,
This is owing to nanoscale humic acid improves crop root surrounding, enhances the root system absorbability to Quadrafos；
(6) the nutrient utilization rate, in the nitrophosphate fertilizer of the present invention is high, and fertilizer is good, and the absorbance of available phosphorus improves, and executes
Being used on crop, crop growing state is more excellent.
Accompanying drawing explanation
Fig. 1 is existing process route chart.
Fig. 2 is present invention process route map.
Detailed description of the invention
Embodiment 1 is containing Quadrafos and the preparation of the nitrophosphate fertilizer A of various nutrient elements
A kind of preparation method containing Quadrafos and the nitrophosphate fertilizer of various nutrient elements is as in figure 2 it is shown, comprise the following steps:
(1) with 5kg nitric acid and 5kg phosphoric acid mixed decomposition 100kg apatite；
(2) ammonia is neutralized to pH is 6.8；
(3) 10kg potassium salt is added；
(4) pressure is down to-0.05MPa and is evaporated concentration, is concentrated to water content 1% weight；
(5) temperature is more than 170 DEG C, is pressurized to 101.32kPa and polyreaction occurs, react 2 hours, generate polyphosphoric acid
Salt；
(6) 5kg nano material is added in Quadrafos, then carry out pelletize and obtain containing Quadrafos and various nutrient elements
Nitrophosphate fertilizer A；
Described nano material is 1.5kg humic acid and utilizes sand milling mach 1kg stone powder, 1kg kieselguhr, 1.5kg magnesite
Ore deposit, the particle diameter of nano material is between 80～100nm.
Embodiment 2 is containing Quadrafos and the preparation of the nitrophosphate fertilizer B of various nutrient elements
A kind of containing Quadrafos and the preparation method of the nitrophosphate fertilizer of various nutrient elements, it is also possible to comprise the following steps:
(1) with 8kg nitric acid and 5kg phosphoric acid mixed decomposition 150kg apatite；
(2) ammonia is neutralized to pH is 6.8；
(3) 15kg potassium salt is added；
(4) pressure is down to-0.05MPa and is evaporated concentration, is concentrated to water content 1% weight；
(5) 6kg nano material being added in concentrated solution, temperature is 170 DEG C, is pressurized to 130kPa and polyreaction occurs, instead
Answer 2 hours, generate containing Quadrafos and the nitrophosphate fertilizer B of various nutrient elements.
Described nano material is 2kg humic acid and utilizes sand milling mach 1kg kieselguhr, 1.5kg bentonite, 1.5kg Pedicellus et Pericarpium Trapae
Magnesium ore deposit, the particle diameter of nano material is in 80～100nm.
Comparative example 1
As different from Example 1, being pressurized to 90.087kPa in comparative example 1 step (5), reaction temperature is 170 DEG C, instead
Answer 2 hours, generate nitrophosphate fertilizer 1.
Comparative example 2
As different from Example 1, in comparative example 2 step (5), pressure remains-0.05MPa, and reaction temperature is 170 DEG C,
React 2 hours, generate nitrophosphate fertilizer 2.
Comparative example 3
As different from Example 1, being pressurized to 55.32kPa in comparative example 3 step (5), reaction temperature is 108 DEG C, instead
Answer 2 hours, generate nitrophosphate fertilizer 3.
Comparative example 4
As different from Example 1, the humic acid in comparative example 4 is not nano level, but replaces with common humic acid,
Other processes are constant, generate nitrophosphate fertilizer 4.
Effect example 1
The content of Quadrafos prepared by the employing paper chromatography each embodiment of analysis and comparative example, the content of Quadrafos in table 1
Computational methods are: Quadrafos wt%=(pyrophosphate+tripolyphosphate+high polymer)/(pyrophosphate+tripolyphosphate+
High polymer+orthophosphate), result such as table 1 below:
Table 1
From table 1, the content of Quadrafos is it can be seen that the content in the nitrophosphate fertilizer prepared of embodiment 1-2 is higher than comparative example,
The pressure and temperature of this explanation embodiment 1-2 is more favourable to the degree of polymerization improving Quadrafos, and generation Quadrafos preferably is poly-
Right higher.
Effect example 2
Nitrophosphate fertilizer 4 prepared by nitrophosphate fertilizer A embodiment 1 prepared and comparative example 4 is applied in cucumber crop soil,
This time test is Fructus Cucumidis sativi pot experiment, arranges a blank potted plant experiment without cucumber crop, potted plant in the soil texture identical,
The cucumber crop root system absorbance to nitrophosphate fertilizer nutrient substance before and after detection fortnight, absorbance is by detection embodiment 1
With the Fructus Cucumidis sativi of comparative example 4 potted plant in nutrient substance (calcium, silicon, magnesium, phosphorus) content reduce relative to content in blank assay
Rate determines, last testing result be embodiment 1 absorbance be 46%, and the absorbance of comparative example 4 is 22%, this explanation
Use nanoscale humic acid that the raising of the absorption of nutrient ingredients utilization rate in nitrophosphate fertilizer is had good effect.
Effect example 3
Being administered on rice crop by nitrophosphate fertilizer prepared by embodiment 1-2 and comparative example 1-4, embodiment 1-2 effect of increasing production shows
Writing, yield averagely improves 15.88%, and in product, calcium averagely improves 12.31%, and silicon averagely improves 19.68%, and comparative example 1-4
Effect of increasing production and rice quality be below embodiment 1-2.
The announcement of book and teaching according to the above description, above-mentioned embodiment can also be entered by those skilled in the art in the invention
Row change and amendment.Therefore, the invention is not limited in detailed description of the invention disclosed and described above, to the present invention
A little modifications and changes should also be as falling in the scope of the claims of the present invention.Although additionally, this specification employing
Some specific terms, but these terms are merely for convenience of description, and the present invention does not constitute any restriction.
Claims (7)
1., containing Quadrafos and a preparation method for the nitrophosphate fertilizer of various nutrient elements, comprise the following steps: (1) uses nitre
Acid and phosphoric acid mixed decomposition apatite；(2) ammonia neutralizes；(3) potassium salt is added；It is characterized in that, also include:
(3) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(4) temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction to generate Quadrafos；
(5) nano material is added in Quadrafos, then carry out pelletize and obtain the nitre containing Quadrafos and various nutrient elements
Acid phosphate fertilizer.
2., containing Quadrafos and a preparation method for the nitrophosphate fertilizer of various nutrient elements, comprise the following steps: (1) uses nitre
Acid and phosphoric acid mixed decomposition apatite；(2) ammonia neutralizes；(3) potassium salt is added；It is characterized in that, also include:
(4) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(5) adding nano material, temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction to generate containing poly-phosphorus
Hydrochlorate and the nitrophosphate fertilizer of multiple nutritional components.
Preparation method the most according to claim 1 and 2, it is characterised in that described nano material comprises nano-sized carbon or receives
Rice humic acid and stone powder, kieselguhr, bentonite, four kinds of ore materials of magnesite in one or more, mean diameter is less than
100nm。
Preparation method the most according to claim 1 and 2, it is characterised in that normal pressure or distillation under pressure process can make
It is condensed between reactant, obtains Quadrafos.
Preparation method the most according to claim 3, it is characterised in that the particle diameter of described nano material is 10～100nm.
6. one kind contains Quadrafos and the nitrophosphate fertilizer of various nutrient elements, it is characterised in that the preparation side of described nitrophosphate fertilizer
Method is as follows:
(1) with nitric acid and phosphoric acid mixed decomposition apatite；
(2) ammonia neutralizes；
(3) potassium salt is added；
(3) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(4) temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction to generate Quadrafos；
(5) nano material is added in Quadrafos, then carry out pelletize and obtain the nitre containing Quadrafos and various nutrient elements
Acid phosphate fertilizer；
Described nano material comprises nano-sized carbon or nanometer humic acid and stone powder, kieselguhr, bentonite, four kinds of Ore materials of magnesite
One or more in material, mean diameter is less than 100nm.
7. one kind contains Quadrafos and the nitrophosphate fertilizer of various nutrient elements, it is characterised in that the preparation side of described nitrophosphate fertilizer
Method is as follows:
(1) with nitric acid and phosphoric acid mixed decomposition apatite；
(2) ammonia neutralizes；
(3) potassium salt is added；
(4) pressure is down to below-0.05MPa and is evaporated concentration, is concentrated to water content≤2% weight；
(5) adding nano material, temperature is more than 170 DEG C, is pressurized to more than normal pressure and occurs polyreaction to generate containing poly-phosphorus
Hydrochlorate and the nitrophosphate fertilizer of multiple nutritional components；
Described nano material comprises nano-sized carbon or nanometer humic acid and stone powder, kieselguhr, bentonite, four kinds of Ore materials of magnesite
One or more in material, mean diameter is less than 100nm.
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| CN2015101474989 | 2015-03-31 | ||
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365775A (en) * | 2016-08-25 | 2017-02-01 | 西南大学 | Potassium-synergistic vegetable special-use fertilizer and preparation method of same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO20065594L (en) * | 2006-12-05 | 2008-06-06 | Yara Int Asa | Production of NPK or NP material containing polyphosphates. |
| CN104108968A (en) * | 2014-07-04 | 2014-10-22 | 贵州芭田生态工程有限公司 | Granulating method of nitric phosphate |
-
2016
- 2016-03-31 CN CN201610196551.9A patent/CN105859329A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO20065594L (en) * | 2006-12-05 | 2008-06-06 | Yara Int Asa | Production of NPK or NP material containing polyphosphates. |
| CN101595078A (en) * | 2006-12-05 | 2009-12-02 | 亚拉国际有限公司 | The NPK or the NP preparation methods that comprise polyphosphate |
| CN104108968A (en) * | 2014-07-04 | 2014-10-22 | 贵州芭田生态工程有限公司 | Granulating method of nitric phosphate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365775A (en) * | 2016-08-25 | 2017-02-01 | 西南大学 | Potassium-synergistic vegetable special-use fertilizer and preparation method of same |
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