CN106365899B - A kind of method that industrial residue prepares siliceous fertilizer - Google Patents
A kind of method that industrial residue prepares siliceous fertilizer Download PDFInfo
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- CN106365899B CN106365899B CN201610748483.2A CN201610748483A CN106365899B CN 106365899 B CN106365899 B CN 106365899B CN 201610748483 A CN201610748483 A CN 201610748483A CN 106365899 B CN106365899 B CN 106365899B
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- siliceous fertilizer
- industrial residue
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- 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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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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- Organic Chemistry (AREA)
- Soil Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to the technical fields of industrial residue recycling and reusing, disclose a kind of method that industrial residue prepares siliceous fertilizer.Preparation method be by electrolytic manganese residues, flyash, sodium carbonate, sodium hydroxide in planetary ball mill, by ratio of grinding media to material 5-10 g/g, revolving speed 150r/min-250r/min, ball milling 20-60min, it is uniformly mixed, is then placed in microwave high-temperature sintering furnace, control temperature in 750-850 DEG C of calcining 10-60min, after crushed, the siliceous fertilizer based on industrial residue is made.The siliceous fertilizer reaches NY/T797-2004 The Ministry of Agriculture of the People's Republic of China, MOA siliceous fertilizer standard.A large amount of electrolytic manganese residues can be effectively utilized in the present invention, and production procedure is short, easy to operate, turn waste into wealth, and provide an effective way for manganese slag resource utilization.
Description
Technical field
The present invention relates to the technical fields of industrial residue recycling and reusing, and in particular to a kind of industrial residue prepares siliceous fertilizer
Method realizes the harmless treatment of electrolytic manganese residues.
Background technique
Silicon is one of the chief elements in the earth's crust, in the soil mainly with a variety of shapes such as crystalline silicon, amorphous silicon and organosilicon
Formula exists.With the rapid development of modern agricultural technology, researcher has found that amorphous silicon and water-soluble silicon can be mentioned significantly in soil
The yield of high crops, moreover it is possible to improve the performances such as crops resistant to lodging, disease resistance, drought-resistant, and promote the decomposition of organic fertilizer, promote
Into nutrient effective use, the harmful substances such as ferrous and methane are mitigated or eliminated harm, make loosing soil and prevent heavy metal
Pollution and other effects.However the silicon in soil, mainly based on crystalline silicon, only effective silicon existing in soil is difficult to meet farming
The production requirement of object.China is large agricultural country, and through investigating, the Yangtze river basin has 70% soil to lack silicon, Liaodong Peninsula, Huang-Huai-Hai
Area's general soil lacks silicon, therefore exploitation prepares siliceous fertilizer and is particularly important.
Currently, there are mainly two types of the methods of domestic production siliceous fertilizer.One kind be it is artificial synthesized, cost is relatively high;Another kind is adopted
It is process with industrial solid castoff, mainly includes high-speed rail metallurgical slag, phosphoric acid industry waste residue, flyash, gangue, silicon ash
Stone, cullet etc. realize the recycling of resource by suitable technique, are the developing direction of siliceous fertilizer preparation process.
Electrolytic manganese metal slag (hereinafter referred to as are as follows: manganese slag) is after manganese carbonate ore prepares manganese sulfate solution by sulfuric acid process leaching
Remaining acid waste residue, discharge amount is big, and according to statistics, every production 1t manganese metal will generate the manganese slag of 8-9t, and China is mostly electric
The method that Xie Meng enterprise is all made of stockpiling of building a dam does not only take up valuable land resource, and due to cinder field construction or rain drop erosion
The problem of, plurality of heavy metal, ammonia nitrogen can be flowed into surrounding body and soil therewith in slag, cause environmental pollution, be seriously endangered
Therefore periphery safety of human and livestock selects a kind of suitable method imperative using manganese slag.According to investigations, contain in manganese slag organic
Nutrient or substance including matter, ammonium sulfate, manganese, silicon, selenium, ammonia nitrogen, potassium, sodium, iron, boron etc., are necessary to crop production
Nutrient can increase the fertilizer efficiency of soil, promote the growth of crop.If certain processing can be passed through, siliceous fertilizer is made in manganese slag,
The effective recycling for being not only able to achieve manganese slag is utilized with comprehensive resource, and reduces the pollution to environment, generates good economic effect
Benefit, environmental benefit and social benefit.
Currently, having the method that fertilizer is made in electrolytic manganese residues by some document reports, these contents reported in the literature are plucked
It records as follows:
Chinese patent CN102372527A discloses a kind of preparation method of Si-Ca-Zn-S-Mg fertilizer, by industrial manganese slag weight
It is raw material than 55-65%, Iron Ore Powder 3-8%, boron mud 3-8%, ashes 18-22%, zeolite powder, rare-earth original ore, is acidified with sulfuric acid,
Obtain product A;Sulfuric acid acidic phosphorus mine powder obtains B;Humic acid, ammonium sulfate, water three are mixed into ammonification chelating, obtain C;By three kinds
Product and magnesium sulfate mixing are obtained than more comprehensively middle trace-element compound fertilizer.This method mainly uses wet processing, utilizes
A large amount of, middle amount and microelement are combined together, prepare Si-Ca-Zn-S-Mg fertilizer, effectively by manganese slag, ashes, rare-earth original ore etc.
Ground improves utilization rate of fertilizer, has saved the energy, but not silicon in activation electrolytic manganese slag.
Jiang Minglei et al. carried out electrolytic manganese metal slag prepare silicomanganese fertilizer experimental study (nation manganese industry, 2014,32 (2):
16-19), the auxiliary agents, in mass ratio 1.00:0.60:0.15 such as calcium carbonate, sodium carbonate, sodium hydroxide are added in electrolytic manganese residues:
0.10, through high-temperature calcination, the available silicon content of acquisition reaches 6.94%, and obtains available silicon content with Microwave Digestion and reach
8.08%, while water-soluble manganese content, up to 1.51%, solubility in citric acid manganese content meets silicomanganese fertilizer standard up to 5.01%.The technology is adopted
With high-temperature calcination technique and Microwave Digestion refined manganese dioxide slag, silicomanganese fertilizer is prepared, silicon obtains in manganese slag activates to a certain extent, but not
Reach siliceous fertilizer standard.
Zhu Yahong has been carried out electrolytic manganese residues manure resources research on utilization (professional degree, Ningxia University paper, 2015), opinion
Text has investigated electrolytic manganese residues and electrolytic manganese residues and organic-inorganic compound mixed fertilizer to soil physico-chemical property and agricultural product security respectively
It influences.The result shows that application electrolytic manganese residues are better than inorganic fertilizer efficiency is administered alone;It is beautiful after electrolytic manganese residues and organic fertilizer compounding application
Rice dry-matter accumulation amount dramatically increases;After electrolytic manganese residues-inorganic composite mixed fertilizer application, capsicum Vc and solvable sugared content significantly increase
Add;And after electrolytic manganese residues and organic-inorganic compound mixed fertilizer application, promote plant growth and development, foods met food security standard is
The new-type fertilizer resource that can be developed and used.The research using crops are directly applied electrolytic manganese residues and and electrolytic manganese residues with have
Machine-inorganic composite mixed fertilizer method explores the fertilizer efficiency of electrolytic manganese residues, but untreated manganese slag cannot achieve resource and maximize benefit
With.
Wang Jing, agriculture Gui Yin, Du Dongyun et al. have carried out research (the comprehensive benefit of mineral products that manganese leached mud prepares white carbon black and manganese fertilizer
With .2012,6:57-59), paper extracts white carbon black using industrial manganese leached mud as raw material, and water-soluble manganese content is in waste residue
1.6%, solubility in citric acid manganese content is 5.1%, reaches the requirement of manganese fertilizer, and adding HyPerF10 is anticaking agent, is reached in additional amount
To after 0.07%, the anti-caking time gradually extends.Silicon extraction in manganese slag is mainly prepared into white carbon black, manganese reaches manganese fertilizer in waste residue
It is required that but leached using high-concentration sodium hydroxide solution, corrosive equipment, and produce a large amount of lye and need to handle.
In conclusion the technique that existing literature is reported, generally just for water-soluble and solubility in citric acid element straight in manganese slag
Utilization, especially promoter manganese are connect, and resource utilization is not realized to existing silicon a large amount of in slag.And China's soil there is a serious shortage of
Active silicon resource, if the demand agriculturally to siliceous fertilizer can not only be alleviated, and be able to achieve to manganese slag using the silicon resource in manganese slag
Efficient utilization.Therefore, it selects the silicon in a kind of suitable method activation electrolytic manganese slag to prepare siliceous fertilizer to have great importance.
Summary of the invention
For the deficiencies in the prior art, ball milling-microwave coupling technology is utilized the object of the present invention is to provide a kind of
The method of activated industrial preparing silicon fertilizer from waste dregs, siliceous fertilizer fineness (passing through 250 μm of standard screens) >=80% obtained, effective silicon (with
SiO2Meter) content >=20%, the product of moisture content≤3% reaches NY/T797-2004 The Ministry of Agriculture of the People's Republic of China, MOA silicon
Fertile standard.
To realize the above-mentioned technical purpose, the invention adopts the following technical scheme:
Electrolytic manganese residues, flyash, sodium carbonate, sodium hydroxide are pressed matter first by a kind of method that industrial residue prepares siliceous fertilizer
Amount is added in planetary ball mill than 1:0.3-0.5:0.4-0.6:0.1, by ratio of grinding media to material 5-10g/g, revolving speed 150r/min-250r/
Min, ball milling 20-60min, then charges material into porcelain boat, is put into microwave high-temperature sintering furnace, controls temperature in 750-850
DEG C calcining 10-60min, after crushed, be made the siliceous fertilizer based on industrial residue.
The electrolytic manganese residues refer to the acid slag that manganese carbonate ore obtains after sulfuric acid process is soaked, and crushed 100 after drying
Mesh is spare.
The flyash is the solid waste of power plant soot discharge, and heated crushed after being dried is sieved with 100 mesh sieve with spare.
The present invention is compared with existing manganese slag prepares soil fertility quality technology, substantive distinguishing features outstanding and significant progress
It is:
(1) compared with existing technique, the present invention uses ball milling-microwave coupling technology, with conventional high temperature calcining technology phase
Than heating rate is fast, and the reaction time is short, shortens 3-6 times than conventional roasting;
(2) compared with existing manganese slag prepares the treatment process of fertilizer, the effective use of silicon resource in manganese slag is realized, is passed through
After activation in product effective silicon (with SiO2Meter) content >=20%, it is much higher than prior art available silicon content obtained;
(3) compared with existing siliceous fertilizer preparation process, Soluble Manganese, solubility in citric acid manganese are activated in manganese slag, improve fertilizer
Fertilizer efficiency, and the aobvious alkalinity of obtained fertilizer can play the role of improveing acid soil.
Specific embodiment
The present invention is further illustrated by the following example, but is not restricted by the embodiments.Own in the following example
Unless otherwise specified the unit of number, ratio and percentage, refers both to quality.
Electrolytic manganese residues refer to the acid slag that manganese carbonate ore obtains after sulfuric acid process is soaked, and crush sieve with 100 mesh sieve after drying
Spare, component is as shown in table 1.
1 electrolytic manganese residues constituent analysis of table
Flyash is the solid waste of power plant soot discharge, and heated crushed after being dried is sieved with 100 mesh sieve with spare, and component is such as
Shown in table 2.
2 flyash constituent analysis of table
Ingredient | SiO2 | Effective silicon | Al | Fe | Ca | Mg | Na | K |
Content (%) | 56.22 | 1.36 | 5.61 | 4.18 | 4.86 | 1.75 | 2.79 | 1.31 |
Embodiment 1
A kind of method that industrial residue prepares siliceous fertilizer: by electrolytic manganese residues, flyash, sodium carbonate, sodium hydroxide by 1:0.4:
0.6:0.1 ratio is added in planetary ball mill, and by ratio of grinding media to material 5g/g, revolving speed 150r/min, Ball-milling Time 20min is mixed
It closes, the material mixed is fitted into porcelain boat, is put into microwave high-temperature sintering furnace, calcination temperature is 800 DEG C, and calcination time is
30min;After crushed, fineness (by 250 μm of standard screens) >=80% are obtained, effective silicon is (with SiO2Meter) content be 21.05%,
PH is 9.87, the siliceous fertilizer product of moisture content≤3%.
The measuring method of siliceous fertilizer pH are as follows: the measurement of NY/T 1377-2007 soil pH.
Embodiment 2-3 is same.
Embodiment 2
A kind of method that industrial residue prepares siliceous fertilizer: by electrolytic manganese residues, flyash, sodium carbonate, sodium hydroxide by 1:0.3:
0.4:0.1 ratio is added in planetary ball mill, and by ratio of grinding media to material 8g/g, revolving speed 200r/min, Ball-milling Time 40min is mixed
It closes, then the material mixed is fitted into porcelain boat, is put into microwave high-temperature sintering furnace, calcination temperature is 850 DEG C, calcination time
For 10min;After crushed, fineness (by 250 μm of standard screens) >=80% are obtained, effective silicon is (with SiO2Meter) content is
20.59%, pH 10.53, the siliceous fertilizer product of moisture content≤3%.
Embodiment 3
A kind of method that industrial residue prepares siliceous fertilizer: by electrolytic manganese residues, flyash, sodium carbonate, sodium hydroxide by 1:0.5:
0.5:0.1 ratio is added in planetary ball mill, and by ratio of grinding media to material 10g/g, revolving speed 250r/min, Ball-milling Time 60min is mixed
It closes, then the material mixed is fitted into porcelain boat, is put into microwave high-temperature sintering furnace, calcination temperature is 750 DEG C, calcination time
For 60min;After crushed, fineness (by 250 μm of standard screens) >=80% are obtained, effective silicon is (with SiO2Meter) content is
20.19%, pH 8.57, the siliceous fertilizer product of moisture content≤3%.
3 embodiment 1-3 siliceous fertilizer test result of table
The above is better embodiment of the invention, is not intended to restrict the invention, all institutes under thinking of the present invention
The various changes and modifications of work, should be included within the scope of the present invention.
Claims (3)
1. a kind of method that industrial residue prepares siliceous fertilizer, it is characterised in that: by electrolytic manganese residues, flyash, sodium carbonate, sodium hydroxide
In mass ratio 1: 0.3-0.5: 0.4-0.6: 0.1 is added in planetary ball mill, by ratio of grinding media to material 5-10 g/g, revolving speed 150
R/min-250r/min, ball milling 20-60 min, then charges material into porcelain boat, is put into microwave high-temperature sintering furnace, control temperature
Degree is in 750-850 DEG C of calcining 10-60 min, after crushed, the siliceous fertilizer based on industrial residue is made;
Siliceous fertilizer fineness >=80%, effective silicon is with SiO2Count content >=20%, moisture content≤3%;
The fineness refers to through 250 μm of standard screens.
2. the method that industrial residue according to claim 1 prepares siliceous fertilizer, it is characterised in that: the electrolytic manganese residues refer to carbon
The acid slag that sour manganese ore obtains after sulfuric acid process is soaked, crushing sieves with 100 mesh sieve spare after drying.
3. the method that industrial residue according to claim 1 prepares siliceous fertilizer, it is characterised in that: the flyash is power plant's combustion
The solid waste of coal discharge, heated crushed after being dried are sieved with 100 mesh sieve with spare.
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CN108262336B (en) * | 2018-02-24 | 2021-05-14 | 昆明理工大学 | Solidification treatment method for electrolytic manganese slag |
CN109896871B (en) * | 2018-12-06 | 2021-07-06 | 桂林理工大学 | Green silicon fertilizer and preparation method thereof |
CN111018573A (en) * | 2019-12-24 | 2020-04-17 | 江阴硕人节能环保科技有限公司 | Silicon fertilizer and production process thereof |
CN111704905A (en) * | 2020-06-18 | 2020-09-25 | 韶关学院 | Soil remediation agent and preparation method and application thereof |
CN111943730A (en) * | 2020-07-14 | 2020-11-17 | 卢建军 | Preparation process of high-doped fly ash potassium-rich silicon fertilizer |
CN115073228B (en) * | 2021-03-12 | 2024-04-02 | 国家能源投资集团有限责任公司 | Silicon fertilizer and preparation method thereof |
CN115108869B (en) * | 2022-06-15 | 2023-09-26 | 华南理工大学 | Method for producing organic-inorganic compound soil conditioner by using coal gangue and product thereof |
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