CN104628479A - Method for preparing controlled release compound fertilizer through magnesium slag phosphorus acid passivation - Google Patents

Method for preparing controlled release compound fertilizer through magnesium slag phosphorus acid passivation Download PDF

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Publication number
CN104628479A
CN104628479A CN201510066667.6A CN201510066667A CN104628479A CN 104628479 A CN104628479 A CN 104628479A CN 201510066667 A CN201510066667 A CN 201510066667A CN 104628479 A CN104628479 A CN 104628479A
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China
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magnesium
magnesium slag
compound fertilizer
slow
release compound
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CN201510066667.6A
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Chinese (zh)
Inventor
程芳琴
廖洪强
梁鹏翔
范远
李咏玲
郭彦霞
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Shanxi University
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Shanxi University
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Priority to CN201510066667.6A priority Critical patent/CN104628479A/en
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B5/00Thomas phosphate; Other slag phosphates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

The invention provides a method for preparing a controlled release compound fertilizer through magnesium slag phosphorus acid passivation, and relates to magnesium slag comprehensive utilization and preparation of a controlled release compound fertilizer. According to the method, magnesium slags, phosphorus acid, urea and potassium sulphate are used as basic materials, magnesium slag phosphorus acid passivation, quantitative dosing, stirring and mixing, prilling, drying and other processing methods are performed, and the controlled release compound fertilizer which can be used for crop growth is prepared. According to the invention, the characteristic that the magnesium slags are enriched in active magnesium oxide and active magnesium oxide and phosphoric acid are easily subjected to passivation reaction to generate magnesium calcium phosphate is fully utilized. The method not only has the advantages that the cost of raw materials is low, the processing process is relatively simple, and scale and industrial production is easy to realize, but also has the comprehensive advantages of no pollution, energy consumption reduction and high-efficient utilization of magnesium slags.

Description

A kind of magnesium slag phosphorus acid passivation prepares the method for slow-release compound fertilizer
Technical field
The present invention relates to the preparation field of slow-release compound fertilizer, particularly utilize magnesium slag phosphorus acid passivation to prepare the method for slow-releasing composite fertilizer.
Background technology
Magnesium slag produces the byproduct in former magnesium process, is adopt Pidgeon process to produce at the former magnesium of China 95%.MAGNESIUM METAL enterprise often produces 1t crude magnesium, can produce the magnesium slag of 6-10t simultaneously.Along with the develop rapidly of China's Smelting magnesium industry, the quantity discharged of magnesium slag is increasing, and storing up of a large amount of magnesium slag can cause a series of environmental problem.The problems such as the recycling of magnesium slag mainly concentrates on building materials in recent years, coal desulfurization, and the fields such as properties-correcting agent exist utilization ways few, and utilization ratio is low.
The main moiety of magnesium slag is CaO, SiO 2, Fe 2o 3, MgO, Al 2o 3deng.These elements are all the necessary nutritive elements of plant, and wherein element silicon has been proved to be the fourth-largest plant nutrient after N, P, K.Farm crop can promote growing of plant after absorbing silicon, improve photosynthesis, improve crops quality.Magnesium residue heavy metal Leaching test result shows, and Cr is 0.012 ± 0.002mgkg -1, Cu is 0.043 ± 0.004mgkg -1, Zn, Ni are all less than 0.001mgkg -1, Pb is less than 0.01mgkg -1, Cr6+ do not detected, the existence of Cd, As, Hg.The relevant limit value that heavy metal content in Leaching is all starkly lower than " limitation of water-soluble fertilizer mercury, arsenic, cadmium, lead, chromium and assay thereof " (NY 1110-2006), provides possibility with regard to carrying out agricultural resources utilization for magnesium slag like this.The contrast of fertilizer product heavy metal index is as shown in the table.
The research report that magnesium slag is used for preparing fertilizer aspect is less, typical patent documentation is analyzed as follows: application for a patent for invention 201010553703.9 provides a kind of technique utilizing magnesium reducing furnace slag to produce efficient calcium magnesium sulphur silicon fertilizer, it is characterized in that magnesium slag and dilute hydrochloric acid filter after reacting, obtain silica polymer, filtrate is divided into two parts in proportion, a and dilute sulphuric acid fully reacts, evaporative crystallization obtains the mixed crystal of calcium sulfate and magnesium sulfate, and another part direct evaporative crystallization at 100-150 DEG C obtains calcium chloride and magnesium chloride crystal.By silica polymer, the crystal obtained by two parts of filtrates mixes granulation, calcium magnesium sulphur silicon fertilizer.This technological process is more complicated, and needs the energy of at substantial, and cost is higher, causes this technique cannot spread.
Slow release fertilizer can be divided into three kinds: (1) one is low water solubility Organic N compound; (2) another kind is by the fertilizer of physical barrier Co ntrolled release, and coated fertilizer is comparatively conventional; (3) low water solubility mineral compound.The slow release fertilizer sold in the market mainly coated, lapping is divided into two kinds, i.e. inorganic coating material and organic coated material, inorganic coating material source is wide, price is low, but poor flexibility, easily crisp, and slow release effect is limited; Organic coated material slow-release is effective, but price high, not easily degrade, not easily large-scale promotion.
Summary of the invention
The object of the invention is the comprehensive Utilization Ways expanding magnesium slag, provides a kind of magnesium slag phosphorus acid passivation to prepare the method for slow-release compound fertilizer, and the method technique is simple, prepared composite fertilizer is with low cost, environmental protection, had good sustained release effect.
A kind of magnesium slag phosphorus acid passivation provided by the invention prepares the method for slow-release compound fertilizer, comprises the steps:
(1) raw material preparation: respectively magnesium slag, urea, industrial sulphuric acid potassium are carried out grinding and makes powder, compound concentration is that (phosphoric acid solution concentration is too small, can bring more juicy into, affect subsequent granulation for 35%-65% phosphoric acid solution; Concentration is excessive, and reaction is too violent, release amount of heat, and evaporation large quantity of moisture, is also unfavorable for reacting completely and subsequent granulation);
(2) react: the phosphoric acid solution prepared is mixed with magnesium ground-slag end, stirs, carry out acid-base neutralisation reaction, generate calcium magnesium phosphate gelling mineral binder bond, realize the passivation of magnesium slag simultaneously; Described phosphoric acid and magnesium slag mass ratio are that (ratio of phosphoric acid and magnesium slag, should meet 2 conditions to 0.6-1:1 in principle: one is that phosphoric acid add-on will to meet completely and active calcium oxide and the reacting weight needed for activated magnesia in magnesium slag; Two is the Minimum requirements amounts that will meet phosphorus in composite fertilizer);
(3) mixing granulation: respectively urea powder and industrial sulphuric acid potassium powder are joined in calcium magnesium phosphate gelling mineral binder bond, fully mix, and granulation, i.e. obtained magnesium slag phosphorus acid passivation slow-release compound fertilizer.Wherein, relative to total inventory, urea add-on is 35%-45%, and potassium sulfate add-on is 20%-30%.
Described magnesium slag, urea, industrial sulphuric acid potassium powder were the powder of 80 mesh sieves.
Compared with prior art, beneficial effect of the present invention:
1. present invention achieves magnesium slag comprehensive utilization of resources, belong to Green Product; 2. contain the plant-growth desired nutritional elements such as nitrogen, phosphorus, potassium, silicon, calcium, magnesium, sulphur, iron in product simultaneously, be beneficial to plant-growth; 3. raw materials cost is lower, achieves full-inorganic binding agent and prepares slow-release fertilizer, the problems such as the high cost effectively avoiding traditional organic binder bond to cause and contaminated soil; 4. preparation technology is simple, is easy to production application, product had good sustained release effect, is beneficial to again the efficiency utilization realizing fertilizer.
The present invention utilizes magnesium slag and phosphorus acid passivation to prepare slow-release compound fertilizer to have very large economy and environment benefit: the first, and magnesium slag can provide growth and development of plants necessary nutritive element to plant, especially in magnesium slag containing a large amount of SiO 2, the resistance of plant can be improved; The second, improve the utilization ratio of fertilizer, reduce fertilizer loss and widespread pollution from the overuse of fertilizers and pesticides in rural area; 3rd, magnesium slag can be utilized in a large number, realize the high-valued comprehensive utilization of magnesium slag; 4th, reduce the cost of slow release fertilizer, be conducive to the large-area popularization of slow release fertilizer
Accompanying drawing explanation
The cumulative release curve of made magnesium slag base slow-release fertilizer K in Fig. 1 embodiment 1
The cumulative release curve of made magnesium slag base slow-release fertilizer K in Fig. 2 embodiment 2
The cumulative release curve of made magnesium slag base slow-release fertilizer K in Fig. 3 embodiment 3
Embodiment
Embodiment 1:
Take magnesium slag, urea, levigate mistake 80 mesh sieve is for subsequent use respectively for industrial sulphuric acid potassium use minigrinder, the phosphoric acid drawing 11.00mL 85% adds 10mL water diluted for use.The magnesium ground-slag end 20g taking 80 mesh sieves puts into beaker; the phosphoric acid diluted is poured in beaker; magnesium slag and phosphoric acid is made to mix abundant reaction with glass stick rapid stirring; then urea powder 41.04g and the industrial sulphuric acid potassium powder 27.20g of 80 mesh sieves was added; fully mix, in granulating disc, mix granulation.Then drying is taken out, i.e. obtained magnesium slag base slow-release fertilizer.It is 2.60% that water soluble method measures the initial stage release rate that made magnesium slag base slow-release fertilizer sustained release performance obtains potassium, the preparation of 28 days is 65.69%, meet the initial stage nutrient release rate that slow release fertilizer national standard (GB/T 23348-2009) requires and be less than or equal to 15%, within 28 days, accumulative nutrient release rate is no more than 80%, K stripping slow release effect as shown in Figure 1.The initial stage release rate of nitrogen is 3.40%, meets the initial stage nutrient release rate that slow release fertilizer national standard (GB/T 23348-2009) requires and is less than or equal to 15%.
Embodiment 2:
Take a certain amount of magnesium slag, urea, levigate mistake 80 mesh sieve is for subsequent use respectively for industrial sulphuric acid potassium use minigrinder, the phosphoric acid drawing 11.00mL 85% adds 15mL water diluted for use.The magnesium ground-slag end 20g taking 80 mesh sieves puts into beaker; the phosphoric acid diluted is poured in beaker; with glass stick rapid stirring, magnesium slag and phosphoric acid are mixed; then urea powder 41.04g and the industrial sulphuric acid potassium powder 27.20g of 80 mesh sieves was added; fully mix; mix granulation in granulating disc after, i.e. obtained magnesium slag base slow-release compound fertilizer.It is 0.78% that water soluble method measures the initial stage release rate that made magnesium slag base slow-release fertilizer sustained release performance obtains potassium, the preparation of 28 days is 62.06%, meet the initial stage nutrient release rate that slow release fertilizer national standard (GB/T 23348-2009) requires and be less than or equal to 15%, within 28 days, accumulative nutrient release rate is no more than 80%, K stripping slow release effect as shown in Figure 2.The preliminary solubility of nitrogen is 6.64%, meets the initial stage nutrient dissolved percentage that slow release fertilizer national standard (GB/T 23348-2009) requires and is less than or equal to 15%.
Embodiment 3:
Take a certain amount of magnesium slag, urea, levigate mistake 80 mesh sieve is for subsequent use respectively for industrial sulphuric acid potassium use minigrinder, the phosphoric acid drawing 8.75mL 85% adds 10mL water diluted for use.The magnesium ground-slag end 20g taking 80 mesh sieves puts into beaker; the phosphoric acid diluted is poured in beaker; with glass stick rapid stirring, magnesium slag and phosphoric acid are mixed; then urea powder 41.04g and the industrial sulphuric acid potassium powder 27.20g of 80 mesh sieves was added; fully mix; granulation in granulating disc, i.e. obtained magnesium slag base slow-release compound fertilizer.It is 0.67% that water soluble method measures the initial stage release rate that made magnesium slag base slow-release fertilizer sustained release performance obtains potassium, the preparation of 28 days is 70.06%, meet the initial stage nutrient release rate that slow release fertilizer national standard (GB/T 23348-2009) requires and be less than or equal to 15%, within 28 days, accumulative nutrient release rate is no more than 80%, K stripping slow release effect as shown in Figure 3.The preliminary solubility of nitrogen is 2.97%, meets the initial stage nutrient dissolved percentage that slow release fertilizer national standard (GB/T 23348-2009) requires and is less than or equal to 15%.

Claims (5)

1. magnesium slag phosphorus acid passivation prepares a method for slow-release compound fertilizer, it is characterized in that, comprises the steps:
(1) raw material preparation: respectively magnesium slag, urea, industrial sulphuric acid potassium are carried out grinding and makes powder, preparation phosphoric acid solution;
(2) react: the phosphoric acid solution prepared is mixed with magnesium ground-slag end, stirs, carry out acid-base neutralisation reaction, generate calcium magnesium phosphate gelling mineral binder bond;
(3) mixing granulation: respectively urea powder and industrial sulphuric acid potassium powder are joined in calcium magnesium phosphate gelling mineral binder bond, fully mix, and granulation, i.e. obtained magnesium slag phosphorus acid passivation slow-release compound fertilizer.
2. a kind of magnesium slag phosphorus acid passivation as claimed in claim 1 prepares the method for slow-release compound fertilizer, it is characterized in that, the concentration of the phosphoric acid solution in described step (1) is 35%-65%.
3. a kind of magnesium slag phosphorus acid passivation as claimed in claim 1 prepares the method for slow-release compound fertilizer, it is characterized in that, the phosphoric acid in described step (2) and magnesium slag mass ratio are 0.6-1:1.
4. a kind of magnesium slag phosphorus acid passivation as claimed in claim 1 prepares the method for slow-release compound fertilizer, it is characterized in that, the urea add-on in described step (3) is the 35%-45% of total inventory, and potassium sulfate add-on is the 20%-30% of total inventory.
5. a kind of magnesium slag phosphorus acid passivation as claimed in claim 1 prepares the method for slow-release compound fertilizer, it is characterized in that, described magnesium slag, urea, industrial sulphuric acid potassium powder were the powder of 80 mesh sieves.
CN201510066667.6A 2015-02-09 2015-02-09 Method for preparing controlled release compound fertilizer through magnesium slag phosphorus acid passivation Pending CN104628479A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105461431A (en) * 2015-12-07 2016-04-06 山西大学 Slow release compound fertilizer via phosphoric acid passivation of magnesium slag
CN105969392A (en) * 2016-05-13 2016-09-28 宁夏大荣化工冶金有限公司 Acidic soil conditioner and method for promoting yield increment and quality improvement by applying same on rice
CN106008059A (en) * 2016-05-13 2016-10-12 宁夏大荣化工冶金有限公司 Acidic soil conditioner and application method thereof to cadmium reduction of rice

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54111465A (en) * 1978-02-10 1979-08-31 Nippon Chemical Ind Production of fused fertilizer with improved quality
JPS60145981A (en) * 1984-12-06 1985-08-01 日之出化学工業株式会社 Manufacture of silicious fertilizer
JPH03237082A (en) * 1990-02-15 1991-10-22 Japan Metals & Chem Co Ltd Granular phosphatic fertilizer containing humid acid
CN102030566A (en) * 2010-11-22 2011-04-27 北京科技大学 New process for producing efficient calcium magnesium sulphur silicon fertilizer by utilizing slag from magnesium reduction furnace

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54111465A (en) * 1978-02-10 1979-08-31 Nippon Chemical Ind Production of fused fertilizer with improved quality
JPS60145981A (en) * 1984-12-06 1985-08-01 日之出化学工業株式会社 Manufacture of silicious fertilizer
JPH03237082A (en) * 1990-02-15 1991-10-22 Japan Metals & Chem Co Ltd Granular phosphatic fertilizer containing humid acid
CN102030566A (en) * 2010-11-22 2011-04-27 北京科技大学 New process for producing efficient calcium magnesium sulphur silicon fertilizer by utilizing slag from magnesium reduction furnace

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105461431A (en) * 2015-12-07 2016-04-06 山西大学 Slow release compound fertilizer via phosphoric acid passivation of magnesium slag
CN105969392A (en) * 2016-05-13 2016-09-28 宁夏大荣化工冶金有限公司 Acidic soil conditioner and method for promoting yield increment and quality improvement by applying same on rice
CN106008059A (en) * 2016-05-13 2016-10-12 宁夏大荣化工冶金有限公司 Acidic soil conditioner and application method thereof to cadmium reduction of rice
CN106008059B (en) * 2016-05-13 2018-02-09 宁夏大荣化工冶金有限公司 A kind of method that cadmium application drops in acidic soil conditioner on rice

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Application publication date: 20150520