CN115197017A - Preparation process for preparing magnesium-potassium inorganic material compound fertilizer from waste resources - Google Patents
Preparation process for preparing magnesium-potassium inorganic material compound fertilizer from waste resources Download PDFInfo
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- CN115197017A CN115197017A CN202210926713.5A CN202210926713A CN115197017A CN 115197017 A CN115197017 A CN 115197017A CN 202210926713 A CN202210926713 A CN 202210926713A CN 115197017 A CN115197017 A CN 115197017A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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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
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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
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
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Abstract
The invention discloses a preparation process for preparing a magnesium-potassium inorganic material compound fertilizer from waste resources, and relates to the technical field of compound fertilizers. The preparation method comprises the steps of humating straws to obtain humus straw powder, reacting polyethylene glycol with vinyltriethoxysilane to obtain a branched vinyl silicon carbon polymer, polymerizing the humus straw powder, N-methylene bisacrylamide, the branched vinyl silicon carbon polymer and acrylic acid to obtain straw gel, carbonizing air-dried cow dung and treating the obtained product with concentrated nitric acid to obtain carbonized cow dung, repeatedly reacting the carbonized cow dung with glycerol triglycidyl ether and ethylenediamine for three times to obtain third-generation carbonized cow dung, carrying out self-assembly on the straw gel and the third-generation carbonized cow dung to obtain a semi-finished compound fertilizer, and enabling the semi-finished compound fertilizer to absorb water to swell and load magnesium potassium salt and urea to obtain the magnesium potassium inorganic material. The magnesium-potassium inorganic material compound fertilizer prepared by the invention has excellent slow release performance and soil hardening prevention performance.
Description
Technical Field
The invention relates to the technical field of compound fertilizers, in particular to a preparation process for preparing a magnesium-potassium inorganic material compound fertilizer from waste resources.
Background
The compound fertilizer is a chemical fertilizer containing two or more nutrient elements, has the advantages of high nutrient content, few side components, good physical properties and the like, and plays an important role in balancing fertilization, improving the utilization rate of the fertilizer and promoting the high and stable yield of crops. In the production of the compound fertilizer, the nutrient condition of soil is measured by using a soil testing formula, and the application amount, the application period and the application method of fertilizers such as nitrogen, phosphorus, potassium, medium and trace elements are provided on the basis of soil testing and fertilizer field experiments according to the fertilizer requirement rule of crops, the fertilizer supply performance of soil and the fertilizer effect on the basis of reasonable application of the organic fertilizers. Generally speaking, the formula fertilizer is scientifically applied under the guidance of agricultural science and technology personnel. The core of the soil testing and formulated fertilization technology is to adjust and solve the contradiction between the fertilizer requirement of crops and the fertilizer supply of soil.
However, it has some disadvantages, such as that its nutrient proportion is always fixed, and the kinds, amounts and proportions of nutrient elements required for different soils and different crops are various. Therefore, before using, the soil is preferably tested, the texture and the nutrient condition of the field soil are known, and in addition, the better effect can be obtained by the cooperation of the fertilizer unit and the soil. Excessive application of nitrogenous fertilizer, phosphate fertilizer, potash fertilizer and other chemical fertilizers causes pollution to the soil. Chemical fertilizer pollution can cause deterioration of physical properties of soil, cause reduction of soil fertility and soil hardening, increase toxic ingredients in food, feed and drinking water, and cause potential harm to health of people and livestock. Therefore, the compound fertilizer can prevent soil hardening, and the slow release is controllable, which is a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation process for preparing a magnesium-potassium inorganic material compound fertilizer from waste resources, which aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation process for preparing a magnesium-potassium inorganic material compound fertilizer from waste resources is characterized in that the magnesium-potassium inorganic material compound fertilizer is prepared by self-assembling straw gel and third-generation carbonized cow dung to obtain a semi-finished compound fertilizer, and then carrying out swelling loading.
The straw gel is prepared by performing humification on crop straws to obtain humic straw powder, reacting polyethylene glycol with vinyl triethoxysilane to obtain a branched vinyl silicon carbon polymer, and performing photo-initiation polymerization on the humic straw powder, N-methylene bisacrylamide, the branched vinyl silicon carbon polymer and acrylic acid.
As optimization, the third-generation carbonized cattle manure is prepared by heating and carbonizing air-dried cattle manure and processing the air-dried cattle manure with concentrated nitric acid to obtain carbonized cattle manure, and sequentially reacting the carbonized cattle manure with glycerol triglycidyl ether and ethylenediamine for three times.
As optimization, the swelling load is to dissolve potassium chloride, magnesium chloride, potassium phosphate and urea in deionized water to prepare an inorganic fertilizer solution, so that the semi-finished compound fertilizer absorbs water, swells and loads in the inorganic fertilizer solution.
As optimization, the preparation method for preparing the magnesium-potassium inorganic material compound fertilizer by using the waste resources comprises the following preparation steps:
(1) Humation: shearing crop straws to 0.8-1.2 cm long, and mixing with deionized water according to the mass ratio of 1: 8-1: 10, uniformly mixing, placing in a high-pressure reaction kettle, reacting at 180-200 ℃ for 70-80 h, cooling, taking out, washing with deionized water for 3-5 times, drying at 70-80 ℃ for 4-6 h, grinding by using an electric grinder, and sieving by using a 0.25-0.3 mm sieve to obtain humic straw powder;
(2) Photo-initiated polymerization: polyethylene glycol and vinyl triethoxysilane are mixed according to the mass ratio of 1:1.1 to 1:1.3, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.01-0.02 time of that of polyethylene glycol, stirring for 20-30 min at 90-100 ℃ and 300-500 r/min, heating to 130-150 ℃, continuing stirring for 6-8 h, cooling to room temperature, standing for 30-40 min at 50-60 ℃ and 1-2 kPa to prepare a branched vinyl silicon carbon polymer; mixing humic straw mixed liquor, N-methylene bisacrylamide alkali liquor, branched vinyl silicon carbon polymer and acrylic acid according to a mass ratio of 20:15:2:1 to 30:20:3:1, uniformly mixing, adding 2,2-dimethoxy-phenyl ketone with the mass of 0.1-0.3 time of that of acrylic acid, irradiating for 50-60 min under an ultraviolet lamp with the light source distance of 30-35 cm, the power of 1-2 kw and the wavelength of 320-380 nm at the temperature of 20-30 ℃, filtering, washing for 3-5 times by using deionized water, drying for 4-6 h at the temperature of 70-80 ℃, grinding by using an electric grinder, and sieving by using a 0.6-0.8 mm sieve to prepare straw gel;
(3) Carbonizing: placing the air-dried cow dung in a vacuum tube furnace, standing for 20-30 min at 100-120 ℃ in sequence in a nitrogen atmosphere, standing for 40-50 min at 300-400 ℃, standing for 20-30 min at 700-800 ℃, cooling to room temperature, taking out, grinding by using an electric grinder, sieving by using a 0.25-0.3 mm sieve, immersing in concentrated nitric acid with the mass fraction of 60-65%, stirring and reacting for 2-3 h at 70-80 ℃ at 800-1000 r/min, taking out, soaking in deionized water for 8-10 min, filtering, washing for 3-5 times by using absolute ethyl alcohol, and drying for 3-4 h at 60-70 ℃ to obtain carbonized cow dung;
(4) Hyperbranched growth: half-generation carbonized cow dung, ethylenediamine and ammonia water with the mass fraction of 20-30% according to the mass ratio of 2:1:30 to 3:1:40, uniformly mixing, carrying out ultrasonic reaction for 2-3 h at 60-70 ℃ and 30-40 kHz, filtering, washing for 3-5 times by using deionized water, and drying for 3-4 h at 60-70 ℃ to obtain a first generation of carbonized cow dung; repeating the above processes twice to obtain third-generation carbonized cow dung;
(5) Self-assembly: immersing straw gel in deionized water, standing for 30-40 min at 30-40 ℃, adding third-generation carbonized cow dung with the mass of 0.6-0.8 time of that of the straw gel, carrying out ultrasonic treatment at 30-40 ℃ and 30-40 kHz for 50-60 min, filtering, drying for 8-10 h at 50-100 Pa at-10-1 ℃, sieving by a sieve of 2-3 mm, and sieving by a sieve of 0.6-0.8 mm to remove redundant third-generation carbonized cow dung to prepare a semi-finished compound fertilizer;
(6) Swelling and loading: immersing the semi-finished compound fertilizer in an inorganic fertilizer solution, soaking for 4-6 h at 70-80 ℃, filtering, and drying for 8-10 h at-10 to-1 ℃ under 50-100 Pa to obtain the magnesium-potassium inorganic material compound fertilizer.
And (2) as optimization, the crop straws in the step (1) are one or a mixture of rice straws, wheat straws and corn straws.
Optimally, the humic straw mixed solution obtained in the step (2) is prepared by mixing humic straw powder, sodium dodecyl sulfate, polyvinylpyrrolidone and deionized water according to a mass ratio of 6:2:1: 80-8: 2:1:100, mixing evenly to prepare the product; the N, N-methylene bisacrylamide alkaline solution is prepared by mixing ammonium persulfate, N-methylene bisacrylamide and 3-5% by mass of sodium hydroxide solution according to the mass ratio of 1:3:30 to 1:4:40 and mixing them uniformly.
As optimization, the air-dried cow dung obtained in the step (3) can be pig dung, horse dung or sheep dung besides cow dung.
As optimization, the preparation method of the semi-generation carbonized cow dung in the step (4) comprises the following steps: carbonized cow dung, glycerol triglycidyl ether, tetrabutylammonium bromide and N, N-dimethylformamide are mixed according to the mass ratio of 5:2:1:20 to 6:3:1:25, uniformly mixing, stirring and reacting for 2-3 h at 80-90 ℃ at 800-1000 r/min in a nitrogen atmosphere, filtering, washing for 3-5 times by using deionized water, and drying for 3-4 h at 60-70 ℃ to prepare the catalyst.
Preferably, the inorganic fertilizer solution obtained in the step (6) is prepared by mixing potassium chloride, magnesium chloride, potassium phosphate, urea and deionized water according to a mass ratio of 1:1:2:4: 10-1: 1:2:6:12 are mixed evenly to prepare the product.
Compared with the prior art, the invention has the following beneficial effects:
when the waste resources are prepared to prepare the magnesium-potassium inorganic material compound fertilizer, the straw gel and the third-generation carbonized cow dung are self-assembled to obtain a semi-finished compound fertilizer, potassium chloride, magnesium chloride, potassium phosphate and urea are dissolved in deionized water to prepare an inorganic fertilizer solution, and the semi-finished compound fertilizer is prepared by absorbing water, swelling and loading in the inorganic fertilizer solution.
Firstly, humification is carried out on crop straws to obtain humus straw powder, so that the humus straw powder has a large number of hydrophilic groups and macromolecular organic matters are hydrolyzed and broken to form a rich pore structure; humic straw powder, N-methylene bisacrylamide, branched vinyl silicon carbon polymer and acrylic acid are subjected to photo-initiation polymerization to generate straw gel, the polymerization of carbon-carbon double bonds enables the whole straw gel to form a three-dimensional network structure, the branched vinyl silicon carbon polymer participates in the polymerization of the carbon-carbon double bonds, the toughness of the material is improved due to the introduction of silicon chains, the stability of a water-absorbing swelling structure is improved, the water-absorbing swelling effect of the straw gel is reduced due to the fact that the branched vinyl silicon carbon polymer enters air holes of the straw gel in the self-assembly process of third-generation carbonized cow dung can be prevented, the straw gel can generate swelling volume change according to the change of water amount, gaps are generated in soil, the soil hardening prevention performance is improved, when swelling load is carried, the inorganic fertilizer solution is alkaline and high in temperature, polyethylene glycol chain segments in the branched vinyl silicon carbon polymer are hydrolyzed to overflow, swelling spaces and channels are increased, and meanwhile, the generated silicon hydroxyl groups have a good combination effect with metal cations in the inorganic fertilizer solution, so that the buffering is easy, and the slow release performance is improved.
Secondly, the air-dried cow dung is heated, carbonized and treated by concentrated nitric acid to obtain carbonized cow dung, the carbonized cow dung is sequentially reacted with glycerol triglycidyl ether and ethylenediamine for three times to obtain third-generation carbonized cow dung, the surface of the third-generation carbonized cow dung contains a large number of hyperbranched amine branched chains, and the hyperbranched amine branched chains can be adsorbed and combined on the straw gel through static electricity and hydrogen bonds to improve the surface hardness and play a role in protection, meanwhile, the straw gel is subjected to swelling volume change according to the change of water quantity, so that the force can be better transferred to soil through the third-generation carbonized cow dung on the surface, the soil is loosened, the soil hardening prevention performance of the compound fertilizer is improved, the hyperbranched amine branched chains have good adsorption and complexation performance on metal ions, and the water storage of the straw gel inside is combined to achieve the effect of slow release, and the slow release performance of the compound fertilizer is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the method in detail, and the method for testing each index of the magnesium-potassium inorganic material compound fertilizer prepared from the waste resources prepared in the following examples is as follows:
slow release performance: the magnesium-potassium inorganic material compound fertilizer obtained in each example and the comparative example material are same in weight, the same plants with the same size are planted in the same soil, the same manner is adopted for fertilization around the plants, a fertilization circle is formed, the same and proper duration is kept, the initial potassium content of the soil is 100%, and the relative amount of potassium ions in the soil on the inner side and the outer side of the fertilization circle is subjected to liquid chromatography.
The performance of preventing soil hardening is as follows: the magnesium-potassium inorganic material compound fertilizer obtained in each embodiment and comparative example materials are same in weight, and are applied outdoors under the same condition, so that the soil hardening degree is poor after a period of time, and the soil is subdivided to keep loose, primarily hardened, moderately hardened and severely hardened.
Yield per mu increment: the same farmland is divided into equal areas, the magnesium-potassium inorganic material compound fertilizer obtained in each example and a comparative example are applied, and the yield increment per mu is recorded (the yield per mu applied with the common compound fertilizer is 100%).
Example 1
(1) Humation: shearing rice straws to be 0.8cm long, and mixing with deionized water according to a mass ratio of 1:8, uniformly mixing, placing in a high-pressure reaction kettle, reacting at 180 ℃ for 80h, cooling, taking out, washing with deionized water for 3 times, drying at 70 ℃ for 6h, grinding by using an electric grinder, and sieving by using a 0.25mm sieve to obtain humic straw powder;
(2) Photo-initiated polymerization: humic straw powder, lauryl sodium sulfate, polyvinylpyrrolidone and deionized water are mixed according to the mass ratio of 6:2:1:80 evenly mixing to prepare a humic straw mixed solution; ammonium persulfate, N-methylene-bisacrylamide and 3-5% by mass of sodium hydroxide solution are mixed according to the mass ratio of 1:3:30, mixing evenly to prepare N, N-methylene-bisacrylamide alkali liquor; polyethylene glycol and vinyl triethoxysilane in a mass ratio of 1:1.1, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.01 time of that of polyethylene glycol, stirring for 20min at 90 ℃ and 300r/min, heating to 130 ℃, continuing stirring for 8h, cooling to room temperature, and standing for 40min at 50 ℃ and 1kPa to obtain a branched vinyl silicon carbon polymer; mixing humic straw mixed liquor, N-methylene bisacrylamide alkaline liquor, branched vinyl silicon-carbon polymer and acrylic acid according to a mass ratio of 20:15:2:1, uniformly mixing, adding 2,2-dimethoxy-phenyl ketone with the mass of 0.1 time of acrylic acid, irradiating for 50min under an ultraviolet lamp with the light source distance of 30cm, the power of 1kw and the wavelength of 320nm at 20 ℃, filtering, washing for 3 times by deionized water, drying for 6h at 70 ℃, grinding by an electric grinder, and sieving by a 0.6mm sieve to obtain straw gel;
(3) Carbonizing: placing the air-dried cow dung in a vacuum tube furnace, standing at 100 ℃ for 30min, standing at 300 ℃ for 50min, standing at 700 ℃ for 30min, cooling to room temperature, taking out, grinding by using an electric grinder, sieving by using a 0.25mm sieve, immersing in concentrated nitric acid with the mass fraction of 60%, stirring at 70 ℃ and 800r/min for reaction for 3h, taking out, placing in deionized water for soaking for 8min, filtering, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ for 4h to obtain carbonized cow dung;
(4) Hyperbranched growth: carbonized cow dung, glycerol triglycidyl ether, tetrabutylammonium bromide and N, N-dimethylformamide are mixed according to the mass ratio of 5:2:1:20, uniformly mixing, stirring and reacting for 3 hours at 80 ℃ and 800r/min in a nitrogen atmosphere, filtering, washing for 3 times by using deionized water, and drying for 4 hours at 60 ℃ to obtain semi-generation carbonized cow dung; mixing half-generation carbonized cow dung, ethylenediamine and ammonia water with the mass fraction of 20% according to the mass ratio of 2:1:30, uniformly mixing, performing ultrasonic reaction for 3 hours at 60 ℃ and 30kHz, filtering, washing for 3 times by using deionized water, and drying for 4 hours at 60 ℃ to obtain a generation of carbonized cow dung; repeating the above processes twice to obtain third-generation carbonized cow dung;
(5) Self-assembly: immersing the straw gel in deionized water, standing for 30min at 30 ℃, adding third-generation carbonized cow dung with the mass 0.6 times that of the straw gel, carrying out ultrasonic treatment for 60min at 30 ℃ and 30kHz, filtering, drying for 10h at-10 ℃ and 50Pa, sieving by a 2mm sieve, and sieving by a 0.6mm sieve to remove the redundant third-generation carbonized cow dung to obtain a semi-finished compound fertilizer;
(6) Swelling and loading: mixing potassium chloride, magnesium chloride, potassium phosphate, urea and deionized water according to a mass ratio of 1:1:2:4:10 mixing evenly to prepare an inorganic fertilizer solution; and immersing the semi-finished product of the compound fertilizer in an inorganic fertilizer solution, soaking for 6 hours at 70 ℃, filtering, and drying for 10 hours at-10 ℃ under 50Pa to obtain the magnesium-potassium inorganic material compound fertilizer.
Example 2
(1) Humification: shearing rice straws to be 1cm long, and mixing the rice straws with deionized water according to a mass ratio of 1:9, uniformly mixing, placing in a high-pressure reaction kettle, reacting at 190 ℃ for 75h, cooling, taking out, washing with deionized water for 4 times, drying at 75 ℃ for 5h, grinding by using an electric grinder, and sieving by using a 0.28mm sieve to obtain humic straw powder;
(2) Photo-initiated polymerization: humic straw powder, sodium dodecyl sulfate, polyvinylpyrrolidone and deionized water are mixed according to the mass ratio of 7:2:1:90 evenly mixing to prepare a humic straw mixed solution; ammonium persulfate, N-methylene-bisacrylamide and a sodium hydroxide solution with the mass fraction of 4% are mixed according to the mass ratio of 1:3:35 mixing evenly to prepare N, N-methylene-bisacrylamide alkali liquor; polyethylene glycol and vinyl triethoxysilane are mixed according to the mass ratio of 1:1.2, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.015 time of that of polyethylene glycol, stirring for 25min at 95 ℃ and 400r/min, heating to 140 ℃, continuing stirring for 7h, cooling to room temperature, and standing for 35min at 55 ℃ and 1.5kPa to obtain a branched vinyl silicon carbon polymer; mixing humic straw mixed liquor, N-methylene bisacrylamide alkaline liquor, branched vinyl silicon-carbon polymer and acrylic acid according to a mass ratio of 25:18:2.5:1, uniformly mixing, adding 2,2-dimethoxy-phenyl ketone with the mass of 0.2 time of acrylic acid, irradiating for 55min under an ultraviolet lamp with the light source distance of 32cm, the power of 1.5kw and the wavelength of 350nm at 25 ℃, filtering, washing for 4 times by deionized water, drying for 5h at 75 ℃, grinding by an electric grinder, and sieving by a 0.7mm sieve to prepare straw gel;
(3) Carbonizing: placing the air-dried cow dung in a vacuum tube furnace, sequentially standing at 110 ℃ for 25min in a nitrogen atmosphere, standing at 350 ℃ for 45min, standing at 750 ℃ for 25min, cooling to room temperature, taking out, grinding by using an electric grinder, sieving by using a 0.28mm sieve, immersing in concentrated nitric acid with the mass fraction of 60%, stirring at 75 ℃ and 900r/min for reaction for 2.5h, taking out, soaking in deionized water for 9min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 3.5h to obtain carbonized cow dung;
(4) Hyperbranched growth: carbonized cow dung, glycerol triglycidyl ether, tetrabutylammonium bromide and N, N-dimethylformamide are mixed according to the mass ratio of 5:2:1:22, uniformly mixing, stirring and reacting for 2.5 hours at 85 ℃ and 900r/min in a nitrogen atmosphere, filtering, washing for 4 times by using deionized water, and drying for 3.5 hours at 65 ℃ to obtain semi-generation carbonized cow dung; mixing half-generation carbonized cow dung, ethylenediamine and 25% ammonia water in a mass ratio of 2:1:35, uniformly mixing, carrying out ultrasonic reaction for 2.5h at 65 ℃ and 35kHz, filtering, washing for 4 times by using deionized water, and drying for 3.5h at 65 ℃ to obtain a generation of carbonized cow dung; repeating the above processes twice to obtain third-generation carbonized cow dung;
(5) Self-assembly: immersing the straw gel in deionized water, standing for 35min at 35 ℃, adding third-generation carbonized cow dung with the mass 0.4 times that of the straw gel, carrying out ultrasonic treatment for 55min at 35 ℃ and 35kHz, filtering, drying for 9h at-5 ℃ and 80Pa, sieving by a 2.5mm sieve, and sieving by a 0.7mm sieve to remove redundant third-generation carbonized cow dung to obtain a semi-finished compound fertilizer;
(6) Swelling and loading: mixing potassium chloride, magnesium chloride, potassium phosphate, urea and deionized water according to a mass ratio of 1:1:2:5:11, uniformly mixing to prepare an inorganic fertilizer solution; and immersing the semi-finished product of the compound fertilizer in an inorganic fertilizer solution, soaking for 5 hours at 75 ℃, filtering, and drying for 9 hours at-5 ℃ under 80Pa to obtain the magnesium-potassium inorganic material compound fertilizer.
Example 3
(1) Humation: shearing rice straws to be 1.2cm long, and mixing the rice straws with deionized water according to the mass ratio of 1:10, uniformly mixing, placing in a high-pressure reaction kettle, reacting at 200 ℃ for 70h, cooling, taking out, washing with deionized water for 5 times, drying at 80 ℃ for 4h, grinding by using an electric grinder, and sieving by using a 0.3mm sieve to obtain humic straw powder;
(2) Photo-initiated polymerization: humic straw powder, lauryl sodium sulfate, polyvinylpyrrolidone and deionized water are mixed according to the mass ratio of 8:2:1:100, evenly mixing to prepare a humic straw mixed solution; ammonium persulfate, N-methylene-bisacrylamide and a sodium hydroxide solution with the mass fraction of 5% are mixed according to the mass ratio of 1:4:40, mixing uniformly to prepare N, N-methylene-bisacrylamide alkali liquor; polyethylene glycol and vinyl triethoxysilane are mixed according to the mass ratio of 1:1.1 to 1:1.3, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.02 time of that of polyethylene glycol, stirring for 20min at 100 ℃ and 500r/min, heating to 150 ℃, continuing stirring for 6h, cooling to room temperature, and standing for 30min at 60 ℃ and 2kPa to obtain a branched vinyl silicon carbon polymer; mixing humic straw mixed liquor, N-methylene bisacrylamide alkali liquor, branched vinyl silicon carbon polymer and acrylic acid according to a mass ratio of 30:20:3:1, uniformly mixing, adding 2,2-dimethoxy-phenyl ketone with the mass of 0.3 time that of acrylic acid, irradiating for 50min under an ultraviolet lamp with the light source distance of 35cm, the power of 2kw and the wavelength of 380nm, filtering, washing for 5 times by deionized water, drying for 4h at 80 ℃, grinding by an electric grinder, and sieving by a 0.8mm sieve to obtain straw gel;
(3) Carbonizing: placing the air-dried cow dung in a vacuum tube furnace, standing for 20min at 120 ℃ in a nitrogen atmosphere, standing for 40min at 400 ℃, standing for 20min at 800 ℃, cooling to room temperature, taking out, grinding by using an electric grinder, sieving by using a 0.3mm sieve, immersing in concentrated nitric acid with the mass fraction of 65%, stirring and reacting for 2h at 80 ℃ and 1000r/min, taking out, placing in deionized water, soaking for 10min, filtering, washing for 5 times by using absolute ethyl alcohol, and drying for 3h at 70 ℃ to obtain carbonized cow dung;
(4) Hyperbranched growth: carbonized cow dung, glycerol triglycidyl ether, tetrabutylammonium bromide and N, N-dimethylformamide are mixed according to the mass ratio of 6:3:1:25, uniformly mixing, stirring and reacting for 2 hours at 90 ℃ and 1000r/min in a nitrogen atmosphere, filtering, washing for 5 times by using deionized water, and drying for 3 hours at 70 ℃ to obtain semi-generation carbonized cow dung; mixing half-generation carbonized cow dung, ethylenediamine and 30% ammonia water in a mass ratio of 3:1:40, uniformly mixing, carrying out ultrasonic reaction for 2 hours at 70 ℃ and 40kHz, filtering, washing for 5 times by using deionized water, and drying for 3 hours at 70 ℃ to obtain a first generation of carbonized cow dung; repeating the above processes twice to obtain third-generation carbonized cow dung;
(5) Self-assembly: immersing the straw gel in deionized water, standing for 30min at 40 ℃, adding third-generation carbonized cow dung with the mass 0.8 times that of the straw gel, carrying out ultrasonic treatment for 50min at 40 ℃ and 40kHz, filtering, drying for 8h at-1 ℃ and 100Pa, sieving by a 3mm sieve, and sieving by a 0.8mm sieve to remove the redundant third-generation carbonized cow dung to obtain a semi-finished compound fertilizer;
(6) Swelling and loading: mixing potassium chloride, magnesium chloride, potassium phosphate, urea and deionized water according to a mass ratio of 1:1:2:6:12 mixing uniformly to prepare an inorganic fertilizer solution; immersing the semi-finished compound fertilizer in an inorganic fertilizer solution, soaking for 4h at 80 ℃, filtering and drying for 8h at-1 ℃ and 100Pa to prepare the magnesium-potassium inorganic material compound fertilizer.
Comparative example 1
The preparation method of the magnesium-potassium inorganic material compound fertilizer using the waste resources of comparative example 1 is different from example 2 only in that step (1) is not performed and step (2) is modified as follows: shearing rice straws to 1cm long, grinding by using an electric grinder, and sieving by using a 0.28mm sieve to obtain straw powder; straw powder, sodium dodecyl sulfate, polyvinylpyrrolidone and deionized water are mixed according to the mass ratio of 7:2:1:90 mixing uniformly to prepare a straw mixed solution; ammonium persulfate, N-methylene-bisacrylamide and a sodium hydroxide solution with the mass fraction of 4% are mixed according to the mass ratio of 1:3:35 evenly mixing to prepare N, N-methylene-bisacrylamide alkali liquor; polyethylene glycol and vinyl triethoxysilane in a mass ratio of 1:1.2, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.015 time of that of polyethylene glycol, stirring for 25min at 95 ℃ and 400r/min, heating to 140 ℃, continuing stirring for 7h, cooling to room temperature, and standing for 35min at 55 ℃ and 1.5kPa to obtain a branched vinyl silicon carbon polymer; mixing straw mixed liquor, N-methylene bisacrylamide alkali liquor, branched vinyl silicon carbon polymer and acrylic acid according to a mass ratio of 25:18:2.5:1, then adding 2,2-dimethoxy-phenyl ketone with the mass of 0.2 time of that of acrylic acid, irradiating for 55min under an ultraviolet lamp with the light source distance of 32cm, the power of 1.5kw and the wavelength of 350nm at the temperature of 25 ℃, filtering, washing for 4 times by deionized water, drying for 5h at the temperature of 75 ℃, grinding by an electric grinder, and sieving by a 0.7mm sieve to prepare the straw gel. The remaining steps were performed in the same manner as in example 2.
Comparative example 2
The preparation method for preparing the magnesium-potassium inorganic material compound fertilizer by using the waste resources of the comparative example 2 is different from the preparation method of the example 2 only in the step (2), and the step (2) is modified as follows: humic straw powder, sodium dodecyl sulfate, polyvinylpyrrolidone and deionized water are mixed according to the mass ratio of 7:2:1:90 evenly mixing to prepare a humic straw mixed solution; ammonium persulfate, N-methylene-bisacrylamide and a sodium hydroxide solution with the mass fraction of 4% are mixed according to the mass ratio of 1:3:35 evenly mixing to prepare N, N-methylene-bisacrylamide alkali liquor; mixing humic straw mixed liquor, N-methylene bisacrylamide alkaline liquor and acrylic acid according to the mass ratio of 25:18:1, then adding 2,2-dimethoxy-phenyl ketone with the mass of 0.2 time of that of acrylic acid, irradiating for 55min under an ultraviolet lamp with the light source distance of 32cm, the power of 1.5kw and the wavelength of 350nm at the temperature of 25 ℃, filtering, washing for 4 times by deionized water, drying for 5h at the temperature of 75 ℃, grinding by an electric grinder, and sieving by a 0.7mm sieve to prepare the straw gel. The remaining steps were performed in the same manner as in example 2.
Comparative example 3
The preparation method of the magnesium-potassium inorganic material compound fertilizer using the waste resources of comparative example 3 is different from example 2 only in that step (4) is not performed and step (5) is modified as follows: immersing the straw gel in deionized water, standing at 35 ℃ for 35min, adding carbonized cow dung with the mass of 0.4 time of that of the straw gel, performing ultrasonic treatment at 35 ℃ and 35kHz for 55min, filtering, drying at-5 ℃ and 80Pa for 9h, sieving by a 2.5mm sieve, and sieving by a 0.7mm sieve to remove redundant carbonized cow dung to obtain the semi-finished compound fertilizer. The remaining steps were performed in the same manner as in example 2.
Comparative example 4
The preparation method for preparing the magnesium-potassium inorganic material compound fertilizer from the waste resources of the comparative example 4 is different from the preparation method of the example 2 only in the difference of the step (6), and the step (6) is modified as follows: mixing: mixing the semi-finished compound fertilizer, potassium chloride, magnesium chloride, potassium phosphate, urea and deionized water according to the mass ratio of 10:1:1:2:5, uniformly mixing to prepare the magnesium-potassium inorganic material compound fertilizer. The remaining steps were performed in the same manner as in example 2.
Examples of effects
The following table 1 shows the performance analysis results of the slow release performance and the soil hardening prevention performance of the magnesium potassium inorganic material compound fertilizer of examples 1 to 3 and comparative examples 1 to 4 of the present invention.
TABLE 1
As can be seen from the comparison of the experimental data of examples 1 to 3 and comparative examples 1 to 4 in Table 1, the magnesium-potassium inorganic material compound fertilizer prepared by the invention has good slow release performance and soil hardening prevention performance.
The experimental data comparison of the examples 1, 2 and 3 and the comparison column 1 shows that the internal potassium ion relative content and the initial hardening of the examples 1, 2 and 3 compared with the comparative example 1 show that the humification is carried out, so that the humified straw powder has a large amount of hydrophilic groups, macromolecular organic matters are hydrolyzed and broken to form rich pore structures, and the effects of good water absorption, water storage and nutrient substance transmission are achieved, and the slow release performance and the soil hardening prevention performance of the magnesium-potassium inorganic material compound fertilizer are improved; from the comparison of experimental data of examples 1, 2 and 3 and comparative example 2, it can be found that the comparative example 2 compared with examples 1, 2 and 3 has relatively high content and moderate hardening of internal potassium ions, which illustrates that the branched vinyl silicon carbon polymer is added in the photo-initiation polymerization process to participate in the polymerization of carbon-carbon double bonds, the introduction of silicon chains increases the toughness of the material, improves the stability of the water-absorbing swelling structure, and can prevent the water-absorbing swelling effect of the straw gel from decreasing due to the air holes entering the straw gel in the third-generation cow dung self-assembly process, so that the straw gel can undergo the change of swelling volume according to the change of water amount, so that the soil crack is generated, thereby improving the soil hardening prevention performance of the magnesium-potassium inorganic material compound fertilizer, when the inorganic fertilizer is subjected to swelling load, the inorganic fertilizer solution becomes alkaline and has higher temperature, the polyethylene glycol chain segment in the branched vinyl silicon carbon polymer is hydrolyzed and overflows, the swelling space and channel are increased, and the generated silicon hydroxyl group has good combination effect with the metal cations in the inorganic fertilizer solution, so that the buffer is easy, thereby improving the slow release performance of the magnesium-potassium inorganic material; the experimental data comparison of examples 1, 2 and 3 and comparative example 3 shows that the internal and external potassium ions in examples 1, 2 and 3 have low and moderate hardening relative to the internal and external potassium ions in comparative example 3, which indicates that hyperbranched growth is performed, the third-generation cattle manure contains a large amount of hyperbranched amine branched chains on the surface, and the hyperbranched amine branched chains can be adsorbed and bonded on straw gel through static electricity and hydrogen bonds, so that the surface hardness is improved and the protection effect is achieved, meanwhile, the straw gel is subjected to the change of swelling volume according to the change of water quantity, and the force can be better transferred to soil through the third-generation cattle manure on the surface to loosen the soil, so that the soil hardening prevention performance of the magnesium-potassium inorganic material compound fertilizer is improved, and the hyperbranched amine branched chains have good adsorption and complexation performance on metal ions and are combined with the straw gel in the interior to store water, so as to achieve the slow release effect, and thus the slow release performance of the magnesium-potassium inorganic material compound fertilizer is improved; from the comparison of the experimental data of the examples 1, 2 and 3 and the comparative example 4, it can be found that the relative contents of the potassium ions measured inside and outside in the examples 1, 2 and 3 and the comparative example 4 are low, which indicates that the inorganic fertilizer can be loaded inside the semi-finished compound fertilizer by performing swelling loading compared with the case of directly mixing, and a large amount of hyperbranched amine branched chains on the surface of the third generation of carbonized cow dung in the semi-finished compound fertilizer can play a good effect of complexing and buffering, so that the inorganic fertilizer is prevented from being dissolved and diffused in the soil, and the slow release performance of the magnesium-potassium inorganic material compound fertilizer is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. A preparation process for preparing a magnesium-potassium inorganic material compound fertilizer from waste resources is characterized in that the magnesium-potassium inorganic material compound fertilizer is prepared by self-assembling straw gel and third-generation carbonized cow dung to obtain a semi-finished compound fertilizer, and then carrying out swelling loading.
2. The preparation process of the magnesium-potassium inorganic material compound fertilizer from the waste resources as claimed in claim 1, wherein the straw gel is prepared by humification of crop straws to obtain humus straw powder, reaction of polyethylene glycol and vinyltriethoxysilane to obtain branched vinyl silicon carbon polymer, and photo-initiation polymerization of the humus straw powder, N-methylenebisacrylamide, branched vinyl silicon carbon polymer and acrylic acid.
3. The process for preparing the magnesium-potassium inorganic material compound fertilizer from the waste resources as claimed in claim 1, wherein the third generation of carbonized cattle manure is prepared by heating, carbonizing and treating with concentrated nitric acid to obtain carbonized cattle manure, and repeatedly reacting the carbonized cattle manure with glycerol triglycidyl ether and ethylenediamine sequentially for three times.
4. The process for preparing the magnesium-potassium inorganic material compound fertilizer by using the waste resources as claimed in claim 1, wherein the swelling load is an inorganic fertilizer solution prepared by dissolving potassium chloride, magnesium chloride, potassium phosphate and urea in deionized water, so that the semi-finished compound fertilizer is subjected to water absorption swelling and loading in the inorganic fertilizer solution.
5. The preparation process for preparing the magnesium-potassium inorganic material compound fertilizer by using the waste resources as claimed in claim 1, which is characterized by comprising the following preparation steps of:
(1) Humation: shearing crop straws to 0.8-1.2 cm long, and mixing with deionized water according to the mass ratio of 1: 8-1: 10, uniformly mixing, placing in a high-pressure reaction kettle, reacting at 180-200 ℃ for 70-80 h, cooling, taking out, washing with deionized water for 3-5 times, drying at 70-80 ℃ for 4-6 h, grinding by using an electric grinder, and sieving by using a 0.25-0.3 mm sieve to obtain humic straw powder;
(2) Photo-initiated polymerization: polyethylene glycol and vinyl triethoxysilane in a mass ratio of 1: 1.1-1: 1.3, uniformly mixing, adding p-toluenesulfonic acid with the mass of 0.01-0.02 time of that of polyethylene glycol, stirring for 20-30 min at 90-100 ℃ and 300-500 r/min, heating to 130-150 ℃, continuing stirring for 6-8 h, cooling to room temperature, standing for 30-40 min at 50-60 ℃ and 1-2 kPa to prepare a branched vinyl silicon carbon polymer; mixing humic straw mixed liquor, N-methylene bisacrylamide alkali liquor, branched vinyl silicon carbon polymer and acrylic acid according to a mass ratio of 20:15:2:1 to 30:20:3:1, uniformly mixing, adding 2,2-dimethoxy-phenyl ketone with the mass of 0.1-0.3 time of that of acrylic acid, irradiating for 50-60 min under an ultraviolet lamp with the light source distance of 30-35 cm, the power of 1-2 kw and the wavelength of 320-380 nm at the temperature of 20-30 ℃, filtering, washing for 3-5 times by using deionized water, drying for 4-6 h at the temperature of 70-80 ℃, grinding by using an electric grinder, and sieving by using a 0.6-0.8 mm sieve to prepare straw gel;
(3) Carbonizing: placing the air-dried cow dung in a vacuum tube furnace, standing for 20-30 min at 100-120 ℃ in sequence in a nitrogen atmosphere, standing for 40-50 min at 300-400 ℃, standing for 20-30 min at 700-800 ℃, cooling to room temperature, taking out, grinding by using an electric grinder, sieving by using a 0.25-0.3 mm sieve, immersing in concentrated nitric acid with the mass fraction of 60-65%, stirring and reacting for 2-3 h at 70-80 ℃ at 800-1000 r/min, taking out, soaking in deionized water for 8-10 min, filtering, washing for 3-5 times by using absolute ethyl alcohol, and drying for 3-4 h at 60-70 ℃ to obtain carbonized cow dung;
(4) Hyperbranched growth: mixing half-generation carbonized cow dung, ethylenediamine and ammonia water with the mass fraction of 20-30% according to the mass ratio of 2:1:30 to 3:1:40, uniformly mixing, carrying out ultrasonic reaction for 2-3 h at the temperature of 60-70 ℃ and the frequency of 30-40 kHz, filtering, washing for 3-5 times by using deionized water, and drying for 3-4 h at the temperature of 60-70 ℃ to obtain a first generation of carbonized cow dung; repeating the above processes twice to obtain third-generation carbonized cow dung;
(5) Self-assembly: immersing straw gel in deionized water, standing for 30-40 min at 30-40 ℃, adding third-generation carbonized cow dung with the mass of 0.6-0.8 time of that of the straw gel, carrying out ultrasonic treatment at 30-40 ℃ and 30-40 kHz for 50-60 min, filtering, drying for 8-10 h at the temperature of-10 to-1 ℃ and 50-100 Pa, sieving by a sieve of 2-3 mm, and sieving by a sieve of 0.6-0.8 mm to remove the redundant third-generation carbonized cow dung to prepare a semi-finished compound fertilizer;
(6) Swelling and loading: immersing the semi-finished compound fertilizer in an inorganic fertilizer solution, soaking for 4-6 h at 70-80 ℃, filtering, and drying for 8-10 h at-10-1 ℃ and 50-100 Pa to prepare the magnesium-potassium inorganic material compound fertilizer.
6. The process for preparing the magnesium-potassium inorganic material compound fertilizer from the waste resources according to claim 5, wherein the crop straws in the step (1) are one or a mixture of rice straws, wheat straws and corn straws.
7. The preparation process of the magnesium-potassium inorganic material compound fertilizer from the waste resources according to claim 5, wherein the humic straw mixed liquor in the step (2) is prepared by mixing humic straw powder, sodium dodecyl sulfate, polyvinylpyrrolidone and deionized water in a mass ratio of 6:2:1: 80-8: 2:1:100, mixing evenly to prepare the product; the N, N-methylene bisacrylamide alkaline solution is prepared by mixing ammonium persulfate, N-methylene bisacrylamide and 3-5% by mass of sodium hydroxide solution according to the mass ratio of 1:3:30 to 1:4:40 and mixing them uniformly.
8. The process for preparing the magnesium-potassium inorganic material compound fertilizer from the waste resources as claimed in claim 5, wherein the air-dried cow dung in the step (3) can be pig dung, horse dung or sheep dung besides cow dung.
9. The preparation process of the magnesium-potassium inorganic material compound fertilizer prepared from the waste resources according to claim 5, wherein the preparation method of the semi-generation carbonized cow dung in the step (4) comprises the following steps: carbonized cow dung, glycerol triglycidyl ether, tetrabutylammonium bromide and N, N-dimethylformamide are mixed according to the mass ratio of 5:2:1:20 to 6:3:1:25, uniformly mixing, stirring and reacting for 2-3 h at 80-90 ℃ at 800-1000 r/min in the nitrogen atmosphere, filtering, washing for 3-5 times by using deionized water, and drying for 3-4 h at 60-70 ℃ to prepare the catalyst.
10. The process for preparing the magnesium-potassium inorganic material compound fertilizer from the waste resources according to claim 5, wherein the inorganic fertilizer solution obtained in the step (6) is prepared by mixing potassium chloride, magnesium chloride, potassium phosphate, urea and deionized water in a mass ratio of 1:1:2:4:10 to 1:1:2:6:12 are mixed evenly to prepare the product.
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