CN112608188A - Preparation method of loess-based geopolymer compound slow-release fertilizer - Google Patents
Preparation method of loess-based geopolymer compound slow-release fertilizer Download PDFInfo
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- CN112608188A CN112608188A CN202110097525.1A CN202110097525A CN112608188A CN 112608188 A CN112608188 A CN 112608188A CN 202110097525 A CN202110097525 A CN 202110097525A CN 112608188 A CN112608188 A CN 112608188A
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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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/006—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mineral polymers, e.g. geopolymers of the Davidovits type
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/10—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
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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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- 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
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/12—Granules or flakes
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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
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/18—Semi-solid fertilisers, e.g. foams or gels
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Abstract
The invention relates to a preparation method of a loess-based geopolymer compound slow-release fertilizer, which comprises the following steps: firstly, alkali is used for exciting loess to polymerize to obtain loess-based open-pore geopolymer; then adding the loess-based open-pore geopolymer into a polyhydroxy high-molecular aqueous solution, stirring, adding a nitrogen fertilizer, continuously stirring in a sealed manner for 0.5-2 h, adding a cross-linking agent solution, and reacting for 3-5 min to obtain a jelly; and (3) injecting the jelly into a gel mold, and drying at 60 ℃ for 36 h to obtain the loess-based geopolymer compound slow-release fertilizer. The loess-based geopolymer compound slow-release fertilizer has the advantages of simple process and low cost, has good slow-release performance and certain water absorption and retention performance, provides a thought and a novel slow-release fertilizer synthesis method for cross-border application in chemistry and agriculture, and has strong practicability and popularization.
Description
Technical Field
The invention relates to the field of agricultural materials and the technical field of composite material science, in particular to a preparation method of a loess-based geopolymer compound slow-release fertilizer.
Background
At present, agricultural production in China depends heavily on chemical fertilizers, but the total utilization rate of nitrogen fertilizers is only 30% -35%, and more than 30% of nitrogen fertilizers are lost by leaching loss, volatilization, surface runoff and the like, and about 30% of nitrogen fertilizers are decomposed and consumed by microorganisms. The excess fertilizer is wasted, the utilization rate of the fertilizer is low, and particularly, the loss is particularly serious when the nitrogen fertilizer is used. The low utilization rate of the fertilizer not only directly causes economic loss, but also causes the problems of surface eutrophication, serious pollution of underground water and the like because the lost fertilizer often enters soil and water bodies. Therefore, the research on the slow release fertilizer has important significance for the development of agricultural industrialization.
The slow release fertilizer is also called slow release fertilizer or controlled release fertilizer, and the release speed of the compound containing nutrients in the fertilizer in soil is slow or the release speed of the nutrients can be controlled to a certain degree for sustained absorption and utilization of crops. The slow release fertilizer can reduce the loss of fertilizer nutrients, particularly nitrogen, in soil, reduce the frequency of fertilization operation, save labor and cost, and avoid the damage to seeds or seedlings caused by excessive fertilization. Therefore, a series of new products of slow and controlled release fertilizers have been developed in succession: such as coated urea, gummy fertilizers, hydrophilic polymer fertilizers and waste plastic film coated fertilizers, biomass coated fertilizers (CN 107473805A), and high polymer slow-release soil improvement materials (CN 105439682A), the above slow-release fertilizers still have many defects: the production cost is too high, the process is complex, the variety and the function are relatively single, the price is too high, the large-area popularization cannot be realized, the sustained and controlled release performance is unstable, or the sustained and controlled release material is difficult to biodegrade in soil, so the popularization and the application of the sustained and controlled release fertilizer are limited. Therefore, the development of novel, efficient, cheap and environment-friendly slow-release fertilizer materials has become the key of the current research.
The geopolymer is an alkali-activated amorphous aluminosilicate material, and compared with the common silicate cementing material, the geopolymer has the advantages of wide raw material source, low cost and little environmental pollution (basically no CO emission)2) Energy conservation, high porosity and the like. Especially the porous structure of the geopolymer can effectively adsorb and fix the carried object in the porous structure. Due to the excellent properties, the research field is greatly widened, and the research is gradually shifted from the conventional experimental preparation to more specific application research, such as the application of the material for fireproof and heat-resistant heat insulation of buildings (CN 105621911A), foaming porous materials, water treatment, air purification, heavy metal solidification, catalyst carriers, nuclear waste sealing and the like. However, the preparation of geopolymer materials is mainly based on clay (such as kaolin), which has high cost, single function and narrow application range.
Loess is a typical natural silicate inorganic mineral raw material, is mainly distributed in latitudinal regions in the world, and occupies an area of 64 km2The structure is loose, porous, uniform in texture and easy to seep water, and is accompanied by a plurality of soluble substances, and the water and soil conservation and vegetation coverage are greatly adversely affected due to the collapsible soil. Therefore, how to realize loess resource utilization is an important research and application direction for curing the polymer. The loess contains SiO as main component2、Al2O3、CaO、Fe2O3And the loess replaces clay minerals to prepare various industrial products, and how to utilize the loess to replace the clay to prepare the geopolymer alkaline cementing material has great practical significance on environmental resources.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a loess-based geopolymer compound slow-release fertilizer with simple process and low cost.
In order to solve the problems, the preparation method of the loess-based geopolymer compound slow-release fertilizer is characterized by comprising the following steps of: firstly, alkali is used for exciting loess to polymerize to obtain loess-based open-pore geopolymer; then adding the loess-based open-pore geopolymer into a polyhydroxy high-molecular water solution, stirring at the speed of 600-1800 r/min for 0.5-3 h, adding a nitrogen fertilizer, continuously stirring in a sealed manner for 0.5-2 h, adding a cross-linking agent solution, and reacting for 3-5 min to obtain a jelly; injecting the jelly into a gel mold, and drying at 60 ℃ for 36 h to obtain the loess-based geopolymer compound slow-release fertilizer; the mass ratio of the nitrogen fertilizer to the loess-based open-cell geopolymer is 1: 1-1: 5; the mass ratio of the cross-linking agent solution to the polyhydroxy high polymer aqueous solution is 1: 1-1: 5.
the loess-based open-pore geopolymer is prepared by the following method:
the method comprises the steps of screening loess particles through a 300-mesh sieve, and drying to obtain dried loess particles;
slowly adding silicate solid in distilled water under magnetic stirring, and stirring at the speed of 400 r/min for 5 min to obtain a colorless solution; adding solid alkali activator, adjusting the rotation speed to 800 r/min, and continuously stirring until the solid alkali activator is dissolved to obtain mixed liquid; the mass ratio of the silicate solid to the dried loess particles is 3-5: 10 to 14; the mass ratio of the dried loess particles to the distilled water is 5-7: 5-6; the mass ratio of the alkali activator solid to the dried loess particles is 0.1-0.5: 10 to 14;
thirdly, adding the dried loess particles into the mixed solution, stirring at room temperature overnight for 8-24 hours, adding a surfactant, increasing the rotating speed to 1000 r/min, and stirring for 10-40 min; then dropwise adding a foaming agent solution, slowing down the foaming amount by controlling the dropwise adding speed, and continuously stirring for 10 min to form uniform turbid liquid; the mass ratio of the surfactant to the dried loess particles is 0.7-0.9: 25-35; the mass ratio of the foaming agent solution to the dried loess particles is 1: 1-1: 35;
and fourthly, injecting the uniform turbid liquid into a mold, and drying at 80 ℃ for 36 hours to obtain the loose porous blocky loess-based open-pore geopolymer.
The silicate solid in the step II is one of sodium silicate, potassium silicate or a mixture of sodium silicate and potassium silicate.
The solid alkali activator in the step II is one of sodium hydroxide, potassium hydroxide or a mixture of sodium hydroxide and potassium hydroxide.
And the surfactant in the step three is one of oleic acid, stearic acid, myristic acid, sunflower oil, soybean oil and Tween-80.
And step three, the foaming agent solution is a solution with the mass concentration of 5-30% which is obtained by dissolving one of hydrogen peroxide, aluminum powder, zinc powder, sodium hypochlorite, sodium perborate, limestone and silica micropowder in water.
Dissolving a polyhydroxy polymer I in distilled water, carrying out water bath at 50-95 ℃ in a constant-temperature magnetic stirrer, stirring for 5-30 min at the rotating speed of 800 r/min until the polyhydroxy polymer I is dissolved, then slowly cooling to 30-70 ℃ in the water bath, adding a polyhydroxy polymer II, and continuously stirring for 8-10 min until the polyhydroxy polymer II is fully dispersed to obtain a viscous polyhydroxy polymer aqueous solution; the mass ratio of the polyhydroxy polymer I to the loess-based open-cell geopolymer is 1: 0.5-1: 10; the mass ratio of the polyhydroxy polymer II to the loess-based open-pore geopolymer is 1: 1-1: 20.
the polyhydroxy polymer I and the polyhydroxy polymer II are respectively one or more of soluble cellulose, carboxymethyl cellulose, hydroxypropyl cellulose, polyvinyl alcohol, starch, sodium alginate, carboxymethyl starch and chitosan.
The nitrogen fertilizer is one of urea, ammonium chloride, ammonium nitrate, ammonium bicarbonate and thiamine.
The cross-linking agent solution is a solution with the mass concentration of 0.5-15% and is prepared by dissolving one of boric acid, N-methylene bisacrylamide and sodium perborate in water.
Compared with the prior art, the invention has the following advantages:
1. the loess-based open-pore geopolymer with a porous structure is obtained by alkali-activated loess polymerization, fertilizer substances are loaded in the pore structure of the loess-based open-pore geopolymer, and an outer layer coating material is formed by using polyhydroxy macromolecules as a crosslinking agent. Compared with pure urea, it has excellent slow releasing performance. Meanwhile, the material has certain water absorption and retention performance due to the gel structure, and is expected to be applied to the field of agricultural planting.
2. The shape and structure of the loess-based geopolymer and loess-based geopolymer compound slow-release fertilizer are analyzed as follows:
loess-based geopolymer and macro-morphology of loess-based geopolymer compound slow-release fertilizer
The macro-morphology of the loess-based geopolymer and the loess-based geopolymer compound slow-release fertilizer prepared by the invention is shown in figure 1. It can be seen that the loess-based geopolymer has a block structure, a large number of pores are formed on the surface, and the loess color of the original loess is also maintained, indicating that the synthetic loess-based open-cell geopolymer is a novel material (fig. 1 a). The loess geopolymer compound slow release fertilizer is in a granular structure, the pore structure of the perforated geopolymer is kept (figure 1 b), the structure of a gel film can be seen from the edge, the gel is coated in the structure of the geopolymer, the porous structure of the loess geopolymer compound slow release fertilizer is favorable for contacting with soil and releasing nutrients, and the slow release gel is favorable for being applied to slow release of the fertilizer.
② the micro-morphology of loess geopolymer and loess geopolymer composite slow-release fertilizer
The microscopic morphology of the prepared loess geopolymer and loess-based geopolymer compound slow-release fertilizer was analyzed by a scanning electron microscope, as shown in fig. 2. FIG. 2a is a loess geopolymer, the surface of which is a porous net-like stacking structure with well-defined edges and obvious pores, which is a typical morphology of geopolymers; fig. 2b shows a loess-based geopolymer compound slow-release fertilizer, which has a plurality of smooth and sticky coatings on the surface, so that the polyhydroxy high-molecular gel is successfully combined with the geopolymer to form the overall appearance of gel, and the successful synthesis of the gel of the geopolymer compound slow-release fertilizer is also proved.
③ loess geopolymer composite slow-release fertilizer infrared spectrogram
As shown in FIG. 3, at 3331, 3207 cm-1The strong peak is attributed to the stretching vibration peak of-OH, which is derived from hydroxyl in polyhydroxy polymer, 2936 cm-1Is due to-CH = OH and 1666 cm-1And 1621 cm-1Two strong peaks are assigned to-C = O peak, are derived from amide group in nitrogen fertilizer, and are at 1026 cm-1The central band belongs TO the antisymmetric stretching vibration of Si (Al) -O-Si and is the typical spectrum of silicate, which is attributed TO TO4（T1/4 : asymmetric stretching vibration of Si or Al) tetrahedron at 755 cm due to polycondensation of alternating Si-O and Al-O bonds-1And 455 cm-1The band at (b) corresponds to the bending vibration peak of Si-O-Si, indicating that the structure of the loess-based geopolymer is retained. In a word, the infrared spectrogram proves the successful synthesis of the loess geopolymer compound slow-release fertilizer.
Map for influence of loess geopolymer compound slow release fertilizer on growth of corn plants
As can be seen from fig. 4, there are, from left to right, a blank group, a control group (commercial compound fertilizer), and four slow-release gel fertilizer groups, wherein the corn plants of the blank group and the commercial fertilizer group are small, while the four groups to which the slow-release gel fertilizer is applied all have good growth vigor, corn leaf width, and plants are large; meanwhile, the four groups added with the slow-release gel fertilizer have large and dense root systems. The slow-release gel fertilizer has a positive promotion effect on the growth of plants and the nourishing of root systems, so that the porous geopolymer slow-release gel fertilizer can be applied to agricultural planting and has a good slow-release effect and a good water retention effect.
Testing water retention performance of loess geopolymer compound slow release fertilizer
Fig. 5 is the water retention performance test results of the geopolymer composite slow release fertilizer and the control (commercial fertilizer) group. From the figure, it can be seen that the trend of the water retention performance of the loess-based geopolymer compound slow-release fertilizer is basically consistent compared with that of the commercial fertilizer group, but the moisture of the commercial fertilizer group is completely lost at the 45 th day, while the loess-based geopolymer compound fertilizer basically loses all the moisture at the 55 th day, and even a small part of the moisture still exists in the geopolymer compound fertilizer. The prepared material has better water retention capacity and can be used for water absorption and retention of soil.
Slow release performance test of loess geopolymer compound slow release fertilizer
The slow release performance of the loess-based geopolymer compound slow release fertilizer can be observed more intuitively and clearly through the quick release of the aqueous solution, so that the aqueous solution is used as a release environment. Respectively weighing a certain amount of geopolymer slow-release fertilizer, taking urea with the same mass as a reference, packaging in a 400-mesh nylon mesh bag, putting into a 500 mL conical flask, adding 250 mL of distilled water, shaking by a shaking table at constant temperature, sampling 5 mL at different time points, and then supplementing with 5 mL of distilled water solution. The absorbance of the released solution was measured by a diacetylmonoxime color development method and the cumulative release rate was calculated, and the experimental results are shown in FIG. 6. The urea reaches the highest release rate at the initial stage of release because the urea is completely dissolved in water and is a single substance, so that the slow release effect is not achieved, and the slow release rate of the geopolymer slow release gel fertilizer is relatively low, so that the geopolymer slow release gel fertilizer has a relatively good slow release effect and is expected to be used as a slow release fertilizer in agricultural planting.
3. The invention fully utilizes a large amount of loess natural resources in China, adopts an alkali excitation method to prepare the geopolymer, is beneficial to saving energy, protecting ecological environment, accords with the strategic target of sustainable development, and can reduce the cost of preparation materials.
4. The method has simple process and low cost, not only provides a new direction for the development and utilization of loess resources and low-cost raw materials of geopolymers, solves the defects of single function and narrow application range of geopolymer materials, but also provides a thought and a novel synthesis method of slow-release fertilizer in the cross-border application of chemistry and agriculture, and has stronger practicability and popularization.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 is a macro-morphology of the loess-based geopolymer and the loess-geopolymer composite slow-release fertilizer of the present invention.
Fig. 2 is a microscopic morphology of the loess-based geopolymer and the loess-geopolymer composite slow-release fertilizer of the present invention.
Fig. 3 is an infrared spectrum of the loess geopolymer compound slow-release fertilizer of the present invention.
FIG. 4 is a diagram showing the effect of the loess geopolymer compound slow-release fertilizer on the growth of corn plants.
FIG. 5 is a water retention property test of the loess geopolymer compound slow-release fertilizer of the present invention.
Fig. 6 is a slow release performance test of the loess geopolymer compound slow release fertilizer of the present invention.
Detailed Description
A preparation method of a loess-based geopolymer compound slow-release fertilizer comprises the following steps: firstly, alkali is used for exciting loess to polymerize to obtain loess-based open-pore geopolymer; then adding a loess-based open-pore geopolymer into a polyhydroxy high-molecular water solution, stirring at the speed of 600-1800 r/min for 0.5-3 h, adding a nitrogen fertilizer, continuously stirring in a sealed manner for 0.5-2 h, adding a cross-linking agent solution, and reacting for 3-5 min to obtain a jelly; and (3) injecting the jelly into a gel mold, and drying at 60 ℃ for 36 h to obtain the loess-based geopolymer compound slow-release fertilizer.
Wherein: the mass ratio of the nitrogen fertilizer to the loess-based open-cell geopolymer is 1: 1-1: 5; the mass ratio of the cross-linking agent solution to the polyhydroxy high polymer aqueous solution is 1: 1-1: 5.
the loess-based open-cell geopolymer is prepared by the following method:
the method comprises the steps of screening loess particles through a 300-mesh sieve, and drying to obtain dried loess particles;
slowly adding silicate solid in distilled water under magnetic stirring, and stirring at the speed of 400 r/min for 5 min to obtain a colorless solution; and adding an alkali activator solid, adjusting the rotation speed to 800 r/min, and continuously stirring until the alkali activator solid is dissolved to obtain a mixed solution. The silicate solid is one of sodium silicate, potassium silicate or a mixture of sodium silicate and potassium silicate. The alkali activator solid is one of sodium hydroxide, potassium hydroxide or a mixture of sodium hydroxide and potassium hydroxide. The mass ratio of the silicate solid to the dried loess particles is 3-5: 10 to 14; the mass ratio of the dried loess particles to the distilled water is 5-7: 5-6; the mass ratio of the solid alkali activator to the dried loess particles is 0.1-0.5: 10 to 14.
Adding dry loess particles into the mixed solution, stirring at room temperature overnight for 8-24 h, adding a surfactant, increasing the rotation speed to 1000 r/min, and stirring for 10-40 min; and then dropwise adding a foaming agent solution, slowing down the foaming amount by controlling the dropwise adding speed, and continuously stirring for 10 min to form uniform turbid liquid. The surfactant is one of oleic acid, stearic acid, myristic acid, sunflower oil, soybean oil and Tween-80. The foaming agent solution is a solution with the mass concentration of 5-30% and is prepared by dissolving one of hydrogen peroxide, aluminum powder, zinc powder, sodium hypochlorite, sodium perborate, limestone and silica micropowder in water. The mass ratio of the surfactant to the dried loess particles is 0.7-0.9: 25-35; the mass ratio of the foaming agent solution to the dried loess particles is 1: 1-1: 35.
and fourthly, injecting the uniform turbid liquid into a mold, and drying at 80 ℃ for 36 hours to obtain the loose porous blocky loess-based open-pore geopolymer.
The polyhydroxy high polymer aqueous solution is prepared by dissolving polyhydroxy high polymer I in distilled water, stirring for 5-30 min in a constant temperature magnetic stirrer in a water bath at 50-95 ℃ at the rotating speed of 800 r/min until the polyhydroxy high polymer I is dissolved, then slowly cooling to 30-70 ℃ in the water bath, adding polyhydroxy high polymer II, and continuously stirring for 8-10 min until the polyhydroxy high polymer I is fully dispersed, thereby obtaining the viscous polyhydroxy high polymer aqueous solution. The polyhydroxy polymer I and the polyhydroxy polymer II are respectively one or more of soluble cellulose, carboxymethyl cellulose, hydroxypropyl cellulose, polyvinyl alcohol, starch, sodium alginate, carboxymethyl starch and chitosan. The mass ratio of the polyhydroxy polymer I to the loess-based open-pore geopolymer is 1: 0.5-1: 10; the mass ratio of the polyhydroxy polymer II to the loess-based open-pore geopolymer is 1: 1-1: 20.
the nitrogen fertilizer is one of urea, ammonium chloride, ammonium nitrate, ammonium bicarbonate and thiamine.
The cross-linking agent solution is a solution with the mass concentration of 0.5-15% and is obtained by dissolving one of boric acid, N-methylene bisacrylamide and sodium perborate in water.
Embodiment 1a preparation method of a loess-based geopolymer compound slow-release fertilizer:
[ PREPARATION OF SOLID-BASED OPEN-PORE GEOLOGICAL POLYMERS ]
First, loess was sieved through a 300-mesh sieve, and dried to prepare 65.0 g of a reaction. Next, 18.000 g of a silicate solid was slowly added to 50 mL of distilled water under magnetic stirring, and stirring was continued (400 r/min) for 5 min to obtain a colorless solution. 2.000 g of alkali activator KOH solid is added, the rotation speed is adjusted to 800 r/min, and then stirring is continued until dissolution. Thirdly, adding 65.0 g of prepared loess, stirring overnight at room temperature for 12 h, adding 1.800 g of surfactant, increasing the rotation speed to 1000 r/min, and stirring for 15 min. 2.4 mL of foaming agent aluminum powder solution (30%) is added dropwise, the foaming amount is reduced by controlling the dropping speed, and then stirring is continued for 10 min to form uniform turbid liquid. And finally, injecting the mixture into a mold, and drying the mixture in an oven at the temperature of 80 ℃ for 36 hours to obtain the loose porous block-shaped loess geopolymer.
[ loess geopolymer compound slow-release fertilizer ]
Weighing 1.200 g of polyvinyl alcohol, dissolving in 60 mL of distilled water, stirring in a constant-temperature magnetic stirrer at a rotating speed of 800 r/min for 15 min at a water bath of 95 ℃ until the polyvinyl alcohol is dissolved, slowly cooling to 65 ℃ and adding 1.800 g of starch, continuously stirring for 8-10 min, adding 4.000 g of the geopolymer, stirring at 1200 r/min to obtain a uniform turbid solution, and continuously stirring for 1.5 h. And then adding 2.000 g of urea, continuously stirring for 1.5 h in a sealed manner, then adding 4 mL of sodium perborate solution, reacting for 3-5 min, injecting the jelly into a gel mold, drying for 36 h in a vacuum oven at 60 ℃, and storing in a drying tower for later use.
The slow release performance of the geopolymer slow release fertilizer reaches 54.6% after 7 d.
Embodiment 2a preparation method of a loess-based geopolymer compound slow-release fertilizer:
[ preparation of loess-based geopolymer ]
First, loess was sieved through a 300-mesh sieve, and dried to prepare 50.0 g of a reaction. Next, 15.000 g of sodium silicate (Na) was slowly added to 50 mL of distilled water under magnetic stirring2SiO3·9H2O) solid, and then stirring (400 r/min) for 5 min to obtain a colorless solution. 2.500 g of solid NaOH as an alkali activator is added, the rotation speed is adjusted to 800 r/min, and then the mixture is continuously stirred until the mixture is dissolved. Thirdly, 50.0 g of prepared loess was added thereto and stirred at room temperature overnight for 16 hours. Adding 1.600 g of cardamom oil, increasing the rotating speed to 1000 r/min, and stirring for 10-20 min. Add dropwise 3.8 mL of blowing agent H2O2The solution (30%) was slowly foamed by controlling the dropping speed, and then stirred for 10 min to form a uniform turbid solution. And finally, injecting into a mold, drying in an oven at 80 ℃ for 36 h to obtain the loose porous block-shaped loess geopolymer, and drying and storing.
[ preparation of loess geopolymer compound slow-release fertilizer ]
Weighing 1.800 g of carboxymethyl cellulose, dissolving the carboxymethyl cellulose in 50 mL of distilled water, stirring the mixture in a constant-temperature magnetic stirrer at a rotating speed of 800 r/min for 15 min at a water bath temperature of 65 ℃ until the carboxymethyl cellulose is dissolved, slowly cooling the mixture to 45 ℃ and adding 1.200 g of sodium alginate into the water bath, continuously stirring the mixture for 8-10 min, adding 5.000 g of the geopolymer, stirring the mixture into uniform turbid liquid at 1200 r/min, and continuously stirring the mixture for 2 h. And then adding 3.000 g of urea, continuously stirring for 1.2 h in a sealed manner, then adding 2 mL of boric acid solution, reacting for 3-5 min, injecting the jelly into a gel mold, drying for 36 h in a vacuum oven at 60 ℃, and storing in a drying tower for later use.
The slow release performance of the geopolymer slow release fertilizer reaches 68.4% after 7 d.
Embodiment 3 a preparation method of a loess-based geopolymer compound slow-release fertilizer:
[ preparation of loess-based geopolymer ]
First, loess was sieved through a 300-mesh sieve, and dried to prepare 50.0 g of a reaction. Next, 18.000 g of potassium silicate solid was slowly added under magnetic stirring in 50 mL of distilled water, followed by further stirring (400 r/min) for 5 min to give a colorless solution. Adding 1.300 g of solid NaOH as alkali activator, adjusting the rotating speed to 800 r/min, and continuing to useStirring until dissolved. Thirdly, 50.0 g of prepared loess was added thereto and stirred at room temperature overnight for 18 hours. Adding 1.400 g of soybean oil, increasing the rotating speed to 1000 r/min, and stirring for 10-20 min. 2.8 mL of blowing agent H was added dropwise2O2The solution (25%) was slowly foamed by controlling the dropping speed, and then stirred for 10 min to form a uniform turbid solution. And finally, injecting into a mold, drying in an oven at 80 ℃ for 36 h to obtain the loose porous block-shaped loess geopolymer, and drying and storing.
[ preparation of loess geopolymer compound slow-release fertilizer ]
Weighing 0.800 g of hydroxypropyl cellulose, dissolving the hydroxypropyl cellulose in 30 mL of distilled water, stirring the mixture in a constant-temperature magnetic stirrer in a 60 ℃ water bath at the rotating speed of 800 r/min for 15 min until the hydroxypropyl cellulose is dissolved, slowly cooling the mixture to 50 ℃ water bath, adding 0.800 g of sodium alginate, continuously stirring the mixture for 8-10 min, adding 2.500 g of the geopolymer, stirring the mixture into uniform turbid liquid at 1200 r/min, and continuously stirring the mixture for 2 h. And then adding 1.800 g of urea, continuously sealing and stirring for 1.8 h, then adding 5 mL of N, N-methylene bisacrylamide solution, reacting for 3-5 min, injecting the jelly into a gel mold, drying for 36 h in a vacuum oven at 60 ℃, and storing in a drying tower for later use.
The slow release performance of the geopolymer slow release fertilizer reaches 58.5% after 7 d.
Embodiment 4 a preparation method of a loess-based geopolymer compound slow-release fertilizer:
[ preparation of loess-based geopolymer ]
First, loess was sieved through a 300-mesh sieve, and dried to prepare 70.0 g of a reaction. Next, 25.000 g of potassium silicate solid was slowly added to 60 mL of distilled water under magnetic stirring, followed by further stirring (400 r/min) for 5 min to give a colorless solution. 0.500 g of solid NaOH as an alkali activator is added, the rotation speed is adjusted to 800 r/min, and then the mixture is continuously stirred until the mixture is dissolved. Thirdly, 70.0 g of prepared loess was added thereto and stirred at room temperature overnight for 18 hours. Adding 1.800 g of oleic acid, increasing the rotating speed to 1000 r/min, and stirring for 10-20 min. 2.1 mL of foaming agent aluminum powder solution (30%) is added dropwise, the foaming amount is reduced by controlling the dropping speed, and then stirring is continued for 10 min to form uniform turbid liquid. And finally, injecting into a mold, drying in an oven at 80 ℃ for 36 h to obtain the loose porous block-shaped loess geopolymer, and drying and storing.
[ preparation of loess geopolymer compound slow-release fertilizer ]
Weighing 1.800 g of hydroxypropyl cellulose, dissolving the hydroxypropyl cellulose in 50 mL of distilled water, stirring the hydroxypropyl cellulose in a constant-temperature magnetic stirrer at the rotating speed of 800 r/min for 15 min at the temperature of 70 ℃ until the hydroxypropyl cellulose is dissolved, slowly cooling the hydroxypropyl cellulose to 60 ℃ in a water bath, adding 1.800 g of starch, continuously stirring for 8-10 min, adding 3.500 g of the geopolymer, stirring the mixture into uniform turbid liquid at the speed of 1200 r/min, and continuously stirring for 1 h. And then adding 2.800 g of urea, continuously stirring for 3 hours in a sealed manner, then adding 2.5 mL of boric acid solution, reacting for 3-5 min, injecting the jelly into a gel mold, drying for 36 hours in a vacuum oven at 60 ℃, and storing in a drying tower for later use.
The slow release performance of the geopolymer slow release fertilizer reaches 46.8% after 7 d.
Claims (10)
1. A preparation method of a loess-based geopolymer compound slow-release fertilizer is characterized by comprising the following steps: firstly, alkali is used for exciting loess to polymerize to obtain loess-based open-pore geopolymer; then adding the loess-based open-pore geopolymer into a polyhydroxy high-molecular water solution, stirring at the speed of 600-1800 r/min for 0.5-3 h, adding a nitrogen fertilizer, continuously stirring in a sealed manner for 0.5-2 h, adding a cross-linking agent solution, and reacting for 3-5 min to obtain a jelly; injecting the jelly into a gel mold, and drying at 60 ℃ for 36 h to obtain the loess-based geopolymer compound slow-release fertilizer; the mass ratio of the nitrogen fertilizer to the loess-based open-cell geopolymer is 1: 1-1: 5; the mass ratio of the cross-linking agent solution to the polyhydroxy high polymer aqueous solution is 1: 1-1: 5.
2. the method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 1, wherein: the loess-based open-pore geopolymer is prepared by the following method:
the method comprises the steps of screening loess particles through a 300-mesh sieve, and drying to obtain dried loess particles;
slowly adding silicate solid in distilled water under magnetic stirring, and stirring at the speed of 400 r/min for 5 min to obtain a colorless solution; adding solid alkali activator, adjusting the rotation speed to 800 r/min, and continuously stirring until the solid alkali activator is dissolved to obtain mixed liquid; the mass ratio of the silicate solid to the dried loess particles is 3-5: 10 to 14; the mass ratio of the dried loess particles to the distilled water is 5-7: 5-6; the mass ratio of the alkali activator solid to the dried loess particles is 0.1-0.5: 10 to 14;
thirdly, adding the dried loess particles into the mixed solution, stirring at room temperature overnight for 8-24 hours, adding a surfactant, increasing the rotating speed to 1000 r/min, and stirring for 10-40 min; then dropwise adding a foaming agent solution, slowing down the foaming amount by controlling the dropwise adding speed, and continuously stirring for 10 min to form uniform turbid liquid; the mass ratio of the surfactant to the dried loess particles is 0.7-0.9: 25-35; the mass ratio of the foaming agent solution to the dried loess particles is 1: 1-1: 35;
and fourthly, injecting the uniform turbid liquid into a mold, and drying at 80 ℃ for 36 hours to obtain the loose porous blocky loess-based open-pore geopolymer.
3. The method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 2, wherein: the silicate solid in the step II is one of sodium silicate, potassium silicate or a mixture of sodium silicate and potassium silicate.
4. The method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 2, wherein: the solid alkali activator in the step II is one of sodium hydroxide, potassium hydroxide or a mixture of sodium hydroxide and potassium hydroxide.
5. The method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 2, wherein: and the surfactant in the step three is one of oleic acid, stearic acid, myristic acid, sunflower oil, soybean oil and Tween-80.
6. The method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 2, wherein: and step three, the foaming agent solution is a solution with the mass concentration of 5-30% which is obtained by dissolving one of hydrogen peroxide, aluminum powder, zinc powder, sodium hypochlorite, sodium perborate, limestone and silica micropowder in water.
7. The method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 1, wherein: dissolving a polyhydroxy polymer I in distilled water, carrying out water bath at 50-95 ℃ in a constant-temperature magnetic stirrer, stirring for 5-30 min at the rotating speed of 800 r/min until the polyhydroxy polymer I is dissolved, then slowly cooling to 30-70 ℃ in the water bath, adding a polyhydroxy polymer II, and continuously stirring for 8-10 min until the polyhydroxy polymer II is fully dispersed to obtain a viscous polyhydroxy polymer aqueous solution; the mass ratio of the polyhydroxy polymer I to the loess-based open-cell geopolymer is 1: 0.5-1: 10; the mass ratio of the polyhydroxy polymer II to the loess-based open-pore geopolymer is 1: 1-1: 20.
8. the method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 7, wherein: the polyhydroxy polymer I and the polyhydroxy polymer II are respectively one or more of soluble cellulose, carboxymethyl cellulose, hydroxypropyl cellulose, polyvinyl alcohol, starch, sodium alginate, carboxymethyl starch and chitosan.
9. The method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 1, wherein: the nitrogen fertilizer is one of urea, ammonium chloride, ammonium nitrate, ammonium bicarbonate and thiamine.
10. The method for preparing a loess-based geopolymer compound slow-release fertilizer as claimed in claim 1, wherein: the cross-linking agent solution is a solution with the mass concentration of 0.5-15% and is prepared by dissolving one of boric acid, N-methylene bisacrylamide and sodium perborate in water.
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