CN114409464A - Preparation method and product of coal gangue compound fertilizer - Google Patents

Preparation method and product of coal gangue compound fertilizer Download PDF

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Publication number
CN114409464A
CN114409464A CN202210048662.0A CN202210048662A CN114409464A CN 114409464 A CN114409464 A CN 114409464A CN 202210048662 A CN202210048662 A CN 202210048662A CN 114409464 A CN114409464 A CN 114409464A
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Prior art keywords
coal gangue
fertilizer
compound fertilizer
preparation
acidic
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Inventor
高成跃
王档良
董青红
翟果果
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Zhongkuang Zhonghe Intelligent Geological Engineering Jiangsu Research Institute Co ltd
China University of Mining and Technology CUMT
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Zhongkuang Zhonghe Intelligent Geological Engineering Jiangsu Research Institute Co ltd
China University of Mining and Technology CUMT
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Priority to CN202210048662.0A priority Critical patent/CN114409464A/en
Publication of CN114409464A publication Critical patent/CN114409464A/en
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B1/00Superphosphates, i.e. fertilisers produced by reacting rock or bone phosphates with sulfuric or phosphoric acid in such amounts and concentrations as to yield solid products directly
    • C05B1/02Superphosphates
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/80Soil conditioners

Abstract

The invention discloses a preparation method of a coal gangue compound fertilizer and a product, belonging to the technical field of solid waste treatment. The preparation steps of the coal gangue compound fertilizer are as follows: dissolving an acidic phosphate fertilizer, an acidic nitrogen fertilizer and potassium permanganate in water, and adding coal gangue particles to obtain a mixture; and carrying out microwave heating on the obtained mixture, and then removing water to obtain the coal gangue compound fertilizer. The invention prepares the gangue compound fertilizer with balanced nutrient elements and high fertilizer efficiency by compounding the acidic phosphate fertilizer, the acidic nitrogen fertilizer, the potassium permanganate and the gangue particles. Through the comprehensive action of all raw materials and preparation steps, the coal gangue solid waste is prepared into the coal gangue compound fertilizer with high fertilizer efficiency, and the reduction and resource utilization of the coal gangue can be realized. Meanwhile, the used raw materials are common raw materials, the preparation steps are simple, the time consumption is short, and the method has high popularization and application values.

Description

Preparation method and product of coal gangue compound fertilizer
Technical Field
The invention relates to the technical field of solid waste treatment, in particular to a preparation method and a product of a coal gangue compound fertilizer.
Background
The coal gangue is a waste generated in the coal mining and processing process and is an industrial solid waste with the largest discharge and stockpiling amount. The stacking of the coal gangue has great influence on the environment, on one hand, the waste of land resources is caused, on the other hand, the weathering and leaching of the coal gangue cause pollution to soil and water, and on the other hand, harmful gas and dust generated by the spontaneous combustion of the coal gangue can also cause pollution to the atmosphere. Therefore, it is necessary to realize the reduction and resource utilization of the coal gangue.
At present, coal gangue is widely used in the fields of power generation, building materials, chemical industry, backfill and agriculture. Since coal gangue is from stratum and has homology with soil, the coal gangue entering the soil as agricultural products is undoubtedly one of the best ways for the effective utilization of the coal gangue.
The development of the coal gangue fertilizer is obviously an effective way, but the coal gangue fertilizer still has a plurality of problems at present, such as: the organic matter in the coal gangue has high solidification degree and low decomposition conversion rate, the effectiveness of a carbon source needs to be improved, nutrient elements are difficult to dissolve out, the nutrient elements are unbalanced, and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a coal gangue compound fertilizer and a product. The coal gangue particles are mixed with the acidic phosphate fertilizer, the acidic nitrogen fertilizer and the potassium permanganate, and then microwave heating is utilized, so that humic acid in the coal gangue particles is oxidized into fulvic acid which is easier to be absorbed by plants, and the organic matter curing degree in the coal gangue particles is reduced; the acidic condition is not only beneficial to the dissolution of nutrient elements (Mg, Mn, Mo, Ca and the like) in the coal gangue particles, but also can enhance the oxidation activity of potassium permanganate; the microwave heating can improve the activity of metal elements in the coal gangue particles, is beneficial to dissolving out the metal elements and can also accelerate the rate of oxidizing humic acid in the coal gangue particles by potassium permanganate; the acidic phosphate fertilizer, the acidic nitrogen fertilizer and the potassium permanganate in the formula can provide more N, P, K for the coal gangue compound fertilizer, and improve the characteristic of uneven nutrient elements of coal gangue particles; manganese in potassium permanganate can be used as a necessary trace element for crop growth, and can inhibit the propagation of harmful bacteria in soil.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention adopts one of the technical schemes: the preparation method of the coal gangue compound fertilizer comprises the following steps:
(1) dissolving an acidic phosphate fertilizer, an acidic nitrogen fertilizer and potassium permanganate in water, and adding coal gangue particles to obtain a mixture;
(2) and (2) carrying out microwave heating on the mixture obtained in the step (1), and then removing moisture to obtain the coal gangue compound fertilizer.
Preferably, the organic content of the coal gangue particles in step (1) is more than 20%.
Preferably, the particle size of the coal gangue particles in the step (1) is less than or equal to 0.8 mm.
Preferably, the mass ratio of the acidic phosphate fertilizer, the acidic nitrogen fertilizer, the potassium permanganate and the coal gangue particles in the step (1) is (0.8-1): 2-3): 0.3-0.5): 10.
Preferably, the mass-volume ratio of the coal gangue particles to the water in the step (1) is 10kg (6-7) L.
In the invention, too little water is not beneficial to mass transfer promotion in the reaction process, and too much water is not beneficial to later-stage water removal.
Preferably, the acidic phosphate fertilizer in step (1) comprises calcium superphosphate and/or ammonium dihydrogen phosphate.
Preferably, the acidic nitrogen fertilizer in step (1) comprises ammonium sulfate and/or ammonium dihydrogen phosphate.
The ammonium dihydrogen phosphate can be used as an acidic phosphate fertilizer and an acidic nitrogen fertilizer. The acidic phosphate fertilizer is a phosphorus-containing fertilizer which is acidic after being dissolved, and the acidic nitrogen fertilizer is a nitrogen-containing fertilizer which is acidic after being dissolved.
Preferably, the microwave heating in the step (2) has microwave power of 900-1000W and time of 30-40 min.
The selected microwave power is too high, so that organic matters in the coal gangue are decomposed, and the fertilizer efficiency is reduced; too low a microwave power will affect the efficiency of the reaction.
The second technical scheme of the invention provides a coal gangue compound fertilizer prepared by the preparation method of the coal gangue compound fertilizer.
The invention has the following beneficial technical effects:
the invention prepares the gangue compound fertilizer with balanced nutrient elements and high fertilizer efficiency by compounding the acidic phosphate fertilizer, the acidic nitrogen fertilizer, the potassium permanganate and the gangue particles.
Specifically, by introducing the acidic phosphate fertilizer and the acidic nitrogen fertilizer, N, P in the coal gangue compound fertilizer is supplemented, and meanwhile, the aqueous solution of the acidic phosphate fertilizer and the acidic nitrogen fertilizer can provide an acidic environment for potassium permanganate, so that the oxidation efficiency of the potassium permanganate is improved; in addition, the acidic condition is also beneficial to dissolving out medium and trace nutrient elements (such as Ca, Mg, Mn, Mo, Ca and the like) in the coal gangue particles, and the fertilizer efficiency is improved.
The potassium permanganate added in the invention can not only provide K element for the coal gangue compound fertilizer, but also oxidize humic acid in coal gangue particles into fulvic acid which is more beneficial to crop absorption through the oxidability of the potassium permanganate, so that the organic matter curing degree in the coal gangue particles is reduced, and the fertilizer efficiency is improved. The manganese element in the potassium permanganate can also inhibit the propagation of harmful bacteria in soil, is also beneficial to the growth of crops and improves the yield of the crops.
The microwave heating is introduced in the preparation process, the reason is that the activity of metal elements in the coal gangue particles can be improved through the microwave treatment, the dissolution efficiency is accelerated by matching with the integral acid environment, and the oxidation efficiency of potassium permanganate can be accelerated by the high temperature generated by the microwave.
The added phosphate fertilizer and nitrogen fertilizer can be kept in a molecular adsorption state by the coal gangue particles, so that the coal gangue particles are easier to absorb by crops, and the effective nutrient content of the coal gangue compound fertilizer is improved.
According to the invention, through the comprehensive action of all raw materials and preparation steps, the coal gangue solid waste is prepared into the coal gangue compound fertilizer with high fertilizer efficiency, and the reduction and resource utilization of the coal gangue can be realized. Meanwhile, the used raw materials are common raw materials, the preparation steps are simple, the time consumption is short, and the method has high popularization and application values.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated value or intervening value in a stated range, and any other stated or intervening value in a stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The invention does not limit the coal gangue and the type, as long as the requirement that the organic matter content of the coal gangue is more than 20 percent is met.
The contents of each component in the coal gangue used in the examples and comparative examples of the present invention are shown in table 1.
TABLE 1
Figure BDA0003473575880000041
Example 1
Preparing a coal gangue compound fertilizer:
(1) crushing the coal gangue, and screening out coal gangue particles with the particle size of less than or equal to 0.8 mm;
(2) taking 10kg of calcium superphosphate, 25kg of ammonium sulfate and 5kg of potassium permanganate, adding 60L of water, adding 100kg of coal gangue particles screened in the step (1) after dissolution, and uniformly stirring to obtain a mixture;
(3) placing the mixture obtained in the step (2) in a microwave heating device, carrying out microwave heating for 40min under the power of 900W to ensure that the reaction is fully carried out, and returning the evaporated moisture in the reaction process to the reactant through a reflux device;
(4) and taking out the reactant after the microwave heating is finished, and placing the reactant in a forced air drying device to evaporate water to dryness to obtain the coal gangue compound fertilizer.
Example 2
Preparing a coal gangue compound fertilizer:
(1) crushing the coal gangue, and screening out coal gangue particles with the particle size of less than or equal to 0.8 mm;
(2) adding 64L of water into 8kg of calcium superphosphate, 30kg of ammonium dihydrogen phosphate and 4kg of potassium permanganate, dissolving, adding 100kg of coal gangue particles sieved in the step (1), and uniformly stirring to obtain a mixture;
(3) placing the mixture obtained in the step (2) in a microwave heating device, carrying out microwave heating for 30min under the power of 100W to fully carry out the reaction, and returning the water evaporated in the reaction process to the reactant through a reflux device;
(4) and taking out the reactant after the microwave heating is finished, and placing the reactant in a forced air drying device to evaporate water to dryness to obtain the coal gangue compound fertilizer.
Example 3
Preparing a coal gangue compound fertilizer:
(1) crushing the coal gangue, and screening out coal gangue particles with the particle size of less than or equal to 0.8 mm;
(2) taking 10kg of calcium superphosphate, 20kg of ammonium dihydrogen phosphate and 4kg of potassium permanganate, adding 64L of water, dissolving, adding 100kg of coal gangue particles sieved in the step (1), and uniformly stirring to obtain a mixture;
(3) placing the mixture obtained in the step (2) in a microwave heating device, carrying out microwave heating for 30min under the power of 100W to fully carry out the reaction, and returning the water evaporated in the reaction process to the reactant through a reflux device;
(4) and taking out the reactant after the microwave heating is finished, and placing the reactant in a forced air drying device to evaporate water to dryness to obtain the coal gangue compound fertilizer.
Example 4
Preparing a coal gangue compound fertilizer:
(1) crushing the coal gangue, and screening out coal gangue particles with the particle size of less than or equal to 0.8 mm;
(2) adding 70L of water into 35kg of ammonium dihydrogen phosphate and 3kg of potassium permanganate, dissolving, adding 100kg of coal gangue particles sieved in the step (1), and uniformly stirring to obtain a mixture;
(3) placing the mixture obtained in the step (2) in a microwave heating device, carrying out microwave heating for 35min under the power of 980W, so that the reaction is fully carried out, and returning the evaporated moisture in the reaction process to the reactant through a reflux device;
(4) and taking out the reactant after the microwave heating is finished, and placing the reactant in a forced air drying device to evaporate water to dryness to obtain the coal gangue compound fertilizer.
Comparative example 1
Preparation of coal gangue compound fertilizer (compared with example 1, microwave heating is changed into heating):
(1) crushing the coal gangue, and screening out coal gangue particles with the particle size of less than or equal to 0.8 mm;
(2) taking 10kg of calcium superphosphate, 25kg of ammonium sulfate and 5kg of potassium permanganate, adding 60L of water, adding 100kg of coal gangue particles screened in the step (1) after dissolution, and uniformly stirring to obtain a mixture;
(3) heating the mixture obtained in the step (2) at 100 ℃ for 8h to fully react, and returning the evaporated moisture in the reaction process to the reactant through a reflux device;
(4) heating and then placing in a blast drying device to evaporate water to obtain the coal gangue compound fertilizer.
Comparative example 2
Preparation of a coal gangue compound fertilizer (compared with example 1, potassium permanganate is replaced by other potassium fertilizers with the same content of K element):
(1) crushing the coal gangue, and screening out coal gangue particles with the particle size of less than or equal to 0.8 mm;
(2) adding 60L of water into 10kg of calcium superphosphate, 25kg of ammonium sulfate and 2.36kg of potassium chloride, dissolving, adding 100kg of coal gangue particles sieved in the step (1), and uniformly stirring to obtain a mixture;
(3) placing the mixture obtained in the step (2) in a microwave heating device, carrying out microwave heating for 40min under the power of 900W to ensure that the reaction is fully carried out, and returning the evaporated moisture in the reaction process to the reactant through a reflux device;
(4) and taking out the reactant after the microwave heating is finished, and placing the reactant in a forced air drying device to evaporate water to dryness to obtain the coal gangue compound fertilizer.
The fertilizer efficiency of the coal gangue compound fertilizer prepared in the examples 1-4 and the comparative examples 1-2 is examined, and the method comprises the following steps:
pupa 857 soybean is selected as a planting crop, sowing is carried out on Xuzhou somewhere in the middle ten days of 4 months, the sowing amount is 4kg per mu, the row spacing is 50cm, the plant spacing is 10cm, 2-3 seeds are planted in each hole, the coal gangue compound fertilizer prepared in the embodiments 1-4 and the comparative examples 1-2 are respectively applied, the fertilizing amount is 15kg per mu, 10kg is used as a base fertilizer and is applied before sowing, 5kg is used as an additional fertilizer and is applied at the beginning of 6 months, the non-fertilization is used as a blank control, and the same field management measures are adopted in each group.
After harvesting, the yield per mu of PuDou 857 soybean applied with different coal gangue compound fertilizers is counted, and the counting result is shown in Table 2.
TABLE 2 yield per mu of Pudou 857 soybeans after application of various sets of coal gangue compound fertilizers
Figure BDA0003473575880000071
Figure BDA0003473575880000081
As can be seen from the table 2, the application of the coal gangue compound fertilizer prepared by the invention can obviously improve the crop yield; under the condition that the common heating means is used for replacing microwave heating in the invention, the fertilizer efficiency of the prepared coal gangue compound fertilizer is obviously reduced (see data of example 1 and comparative example 1), and under the condition that the microwave is omitted, the activity of nutrient elements in the coal gangue is lower, and the nutrient elements which can be absorbed by crops in the prepared compound fertilizer are less, so that the yield is reduced; under the condition that other potassium fertilizers are used for replacing potassium permanganate in the invention, the fertilizer efficiency of the prepared coal gangue compound fertilizer is also reduced (see data of example 1 and comparative example 2), and the necessity of adopting potassium permanganate with oxidability as a raw material of the coal gangue compound fertilizer is proved, and the main function of the fertilizer is to oxidize humic acid in coal gangue into fulvic acid in the preparation process.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (9)

1. The preparation method of the coal gangue compound fertilizer is characterized by comprising the following steps:
(1) dissolving an acidic phosphate fertilizer, an acidic nitrogen fertilizer and potassium permanganate in water, and adding coal gangue particles to obtain a mixture;
(2) and (2) carrying out microwave heating on the mixture obtained in the step (1), and then removing moisture to obtain the coal gangue compound fertilizer.
2. The preparation method of the coal gangue compound fertilizer as defined in claim 1, wherein the organic matter content of the coal gangue particles in the step (1) is more than 20%.
3. The preparation method of the coal gangue compound fertilizer as defined in claim 1, wherein the grain size of the coal gangue particles in step (1) is less than or equal to 0.8 mm.
4. The preparation method of the coal gangue compound fertilizer as defined in claim 1, wherein the mass ratio of the acidic phosphate fertilizer, the acidic nitrogen fertilizer, the potassium permanganate and the coal gangue particles in the step (1) is (0.8-1): (2-3): (0.3-0.5): 10.
5. The preparation method of the coal gangue compound fertilizer as claimed in claim 1, wherein the mass-to-volume ratio of the coal gangue particles to water in the step (1) is 10kg (6-7) L.
6. The method for preparing the coal gangue compound fertilizer as defined in claim 1, wherein the acidic phosphate fertilizer in the step (1) comprises calcium superphosphate and/or ammonium dihydrogen phosphate.
7. The method for preparing a coal gangue compound fertilizer as defined in claim 1, wherein the acidic nitrogen fertilizer in step (1) comprises ammonium sulfate and/or ammonium dihydrogen phosphate.
8. The preparation method of the coal gangue compound fertilizer as defined in claim 1, wherein the microwave heating in the step (2) has a microwave power of 900-1000W and a time of 30-40 min.
9. The coal gangue compound fertilizer prepared by the preparation method of the coal gangue compound fertilizer according to any one of claims 1 to 8.
CN202210048662.0A 2022-01-17 2022-01-17 Preparation method and product of coal gangue compound fertilizer Pending CN114409464A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115448801A (en) * 2022-09-22 2022-12-09 舒新前 Coal-based solid waste humic acid mineral fertilizer and preparation method and application thereof

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CN109988047A (en) * 2019-04-26 2019-07-09 珠海三豫环保新材料科技有限公司 A kind of formula and preparation method thereof preparing mineral composite bacterial fertilizer using gangue
CN110002904A (en) * 2019-04-26 2019-07-12 珠海三豫环保新材料科技有限公司 A kind of formula and preparation method thereof preparing acid soil improving agent using gangue
CN113582763A (en) * 2021-08-18 2021-11-02 中科鼎乾(北京)环保发展有限公司 Method and system for producing high-silicon compound fertilizer by activating coal gangue

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CN1166475A (en) * 1997-04-01 1997-12-03 文晓青 Preparation of humic acid organic fertilizer
CN1229774A (en) * 1999-03-16 1999-09-29 冯月瑛 Humic acid ecological organic fertilizer prepn. method
CN103319213A (en) * 2013-03-05 2013-09-25 西北大学 Method for preparing complex fertilizer by using coal gangue
CN106747680A (en) * 2017-03-10 2017-05-31 湖北民族学院 The preparation method of active element selenium and its selenium fertilizer in a kind of alkaline process active coal gangue
CN107673927A (en) * 2017-11-03 2018-02-09 黑龙江省农业科学院土壤肥料与环境资源研究所 A kind of rice slow-release fertilizer and preparation method thereof
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CN109928836A (en) * 2019-04-26 2019-06-25 珠海三豫环保新材料科技有限公司 A method of mineral organic compound fertilizer is prepared using gangue
CN109988047A (en) * 2019-04-26 2019-07-09 珠海三豫环保新材料科技有限公司 A kind of formula and preparation method thereof preparing mineral composite bacterial fertilizer using gangue
CN110002904A (en) * 2019-04-26 2019-07-12 珠海三豫环保新材料科技有限公司 A kind of formula and preparation method thereof preparing acid soil improving agent using gangue
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115448801A (en) * 2022-09-22 2022-12-09 舒新前 Coal-based solid waste humic acid mineral fertilizer and preparation method and application thereof

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