Organic compound fertilizer and preparation method thereof

Abstract

The invention belongs to the technical field of fertilizers. The invention provides an organic compound fertilizer and a preparation method thereof.The method comprises the steps that S1, corn straw and chicken manure are dried in the sun and smashed, and straw particles and chicken manure particles are obtained; s2, uniformly mixing 18 to 20 parts by weight of the straw particles, 77 to 80 parts by weight of chicken manure particles, 20 to 23 parts by weight of sawdust, 2.5 to 3 parts by weight of a fermentation inoculant, 3.2 to 3.7 parts by weight of hexadecyl trimethyl ammonium chloride modified attapulgite and 3 to 3.5 parts by weight of calcified humic acid so as to obtain a mixture; s3, putting the mixture into a fermentation tank, fermenting for 25-28 days, discharging, and drying to obtain a base fertilizer; and adding a humic acid substance accounting for 2.8-3.2% of the mass of the organic compound fertilizer and polyglutamic acid accounting for 1.8-2.1% of the mass of the organic compound fertilizer, and uniformly mixing to obtain the organic compound fertilizer. By increasing the adding amount of the corn straw, the organic matter content of the prepared organic compound fertilizer is increased, and meanwhile the seed germination rate is further increased.

Description

An organic compound fertilizer and its preparation method Technical Field

[0001] This invention belongs to the field of fertilizer technology, specifically relating to an organic compound fertilizer and its preparation method. Background Technology

[0002] Fertilizer is an essential production material for agriculture and forestry. Long-term application of chemical fertilizers can easily lead to problems such as soil acidification, and the production and application of chemical fertilizers can easily pollute the environment. Although organic wastes generated in daily production and life, such as sludge, livestock and poultry manure, fruit pomace, soy sauce residue, medicinal residue, dead branches and leaves, straw, rice husks, etc., are rich in nitrogen, phosphorus, potassium, amino acids, organic matter, etc., the organic matter exists in the form of cellulose and other substances that crops cannot absorb, and therefore cannot be directly used as fertilizer.

[0003] Current technology involves adding corn stalks and other additives to chicken manure, followed by fermentation to prepare organic compound fertilizer. Because corn stalks contain abundant carbon and nitrogen sources, the organic matter content of the resulting compound fertilizer continuously increases with the amount of corn stalks added. However, excessive addition of corn stalks leads to a decrease in seed germination rate measurements of the resulting organic compound fertilizer. Summary of the Invention

[0004] To address the problems existing in the background technology, this invention proposes an organic compound fertilizer and its preparation method. By increasing the amount of corn stalks added, the organic matter content of the prepared organic compound fertilizer is increased, while the seed germination rate is further improved.

[0005] To achieve the above objectives, in a first aspect, the present invention provides a method for preparing an organic compound fertilizer, comprising the following steps: S1, drying and crushing corn stalks and chicken manure under the sun to obtain stalk granules and chicken manure granules; S2, mixing 18-20 parts by weight of the stalk granules, 77-80 parts by weight of chicken manure granules, 20-23 parts by weight of sawdust, 2.5-3 parts by weight of fermentation agent, 3.2-3.7 parts by weight of hexadecyltrimethylammonium chloride-modified attapulgite, and 3-3.5 parts by weight of calcified humic acid to obtain a mixture; S3, placing the mixture into a fermentation tank, fermenting for 25-28 days, discharging, drying, and obtaining a base fertilizer; adding 2.8-3.2% by weight of humic acid and 1.8-2.1% by weight of polyglutamic acid, mixing well, to obtain the organic compound fertilizer.

[0006] Further, the preparation method of the hexadecyltrimethylammonium chloride modified attapulgite is as follows: A1. Attapulgite is treated with hydrochloric acid solution, filtered, washed, and dried to obtain pretreated attapulgite; A2. The pretreated attapulgite obtained in A1 is treated with sodium chloride solution, filtered, washed, and dried to obtain sodium-modified attapulgite; A3. The sodium-modified attapulgite obtained in A2 is mixed with hexadecyltrimethylammonium chloride at a mass ratio of 3:1, ultrasonicated for 20 min, and stirred at 70±5℃ for 4-4.5 h. After the reaction is complete, a mixture is obtained. The mixture is cooled to room temperature, filtered, and washed until chloride ions are no longer detectable in the filtrate. Then it is dried at 80℃ to obtain the hexadecyltrimethylammonium chloride modified attapulgite.

[0007] Further, the specific operation of A1 is as follows: attapulgite is mixed with hydrochloric acid solution with a concentration of 1±0.1mol / L at a ratio of 1g:(3.5-4.5)mL, and stirred to remove some large particles and cations outside the structure in the raw ore. After stirring for 120-150min, the suspension is filtered, washed until neutral, dried, and pulverized to obtain pretreated attapulgite.

[0008] Further, the specific operation of A2 is as follows: the pretreated attapulgite obtained from A1 is mixed with a sodium chloride solution with a concentration of 1±0.1mol / L at a ratio of 1g:(12-14)mL, stirred at 40±2℃ for 45-48h, filtered, and washed with deionized water until no chloride ions are detected in the filtrate with 0.1mol / L silver nitrate; then dried at 80℃ and ground to obtain sodium-treated attapulgite.

[0009] Further, the preparation method of the calcified humic acid is as follows: B1. After pulverizing the humic acid, calcine it in a muffle furnace and cool it to obtain calcined powder; B2. First, soak the calcined powder obtained in B1 in calcium chloride solution for 2-2.5 hours and then filter it; then soak it in sodium nitrate solution for 5-8 minutes and filter it; wash it with water and filter it (soak and filter it in distilled water multiple times), and dry it to obtain the calcified humic acid.

[0010] Furthermore, in B1, the calcination temperature is 370-400℃ and the calcination time is 1-1.2h.

[0011] Further, in B2, the concentration of the calcium chloride solution is 2 ± 0.1 mol / L; and the concentration of the sodium nitrate solution is 1 ± 0.1 mol / L.

[0012] Furthermore, in S1, the particle size of the straw pellets and chicken manure pellets does not exceed 40 mesh.

[0013] Furthermore, in S2, the fermentation agent includes Bacillus subtilis, Bacillus licheniformis, Trichoderma harzianum, Aspergillus oryzae, and Rhodotorula rubra.

[0014] Secondly, the present invention provides an organic compound fertilizer prepared by the above-described preparation method.

[0015] This application has the following beneficial effects: In the preparation of organic compound fertilizer of the present invention, when calcified humic acid and hexadecyltrimethylammonium chloride modified attapulgite are introduced at the same time, on the one hand, calcified humic acid and hexadecyltrimethylammonium chloride modified attapulgite form a composite structure through calcium bridge bonding, which is conducive to increasing oxygen transport efficiency and aerobic bacteria proliferation, effectively weakening / counteracting the negative effects brought about by introducing hexadecyltrimethylammonium chloride modified attapulgite alone.

[0016] On the other hand, in the early stage, hexadecyltrimethylammonium chloride-modified attapulgite rapidly adsorbs free ammonium, avoiding early ammonia volatilization; in the middle stage, calcified humic acid slowly releases Ca. 2+ Activates urease, promoting the adsorption of NH4 + Directed conversion to NO3 - Later, as the nitrifying bacteria community matures, nitrogen utilization significantly improves, thus achieving a synergistic effect of increasing seed germination rate. Attached Figure Description

[0017] Figure 1 is a comparative trend chart of the organic matter and seed germination rate measurement data of the organic compound fertilizers prepared in Examples 1-3 and Comparative Examples 1-3 of the present invention. Detailed Implementation

[0018] The present application will be further described in detail below with reference to the embodiments.

[0019] Unless otherwise specified, the raw materials used in the embodiments and comparative examples of this application are all commercially available.

[0020] Example 1: (a) Preparation of hexadecyltrimethylammonium chloride modified attapulgite, the preparation method is as follows: A1. Attapulgite is mixed with hydrochloric acid solution with a concentration of 1 mol / L at a ratio of 1 g: 4 mL. At room temperature, the mixture is continuously stirred at a stirring speed of 300 r / min to remove some large particles and cations outside the structure in the raw ore. After stirring for 130 min, the suspension is filtered and repeatedly washed with deionized water until the pH of the filtrate is neutral at 7. Then, it is placed in an electric heating drying oven with the temperature set at 105℃ and the drying time at 6 h to dry it. Then, it is pulverized to a particle size that passes through a 200 mesh sieve to obtain pretreated attapulgite.

[0021] A2. The pretreated attapulgite obtained in A1 was mixed with a 1 mol / L sodium chloride solution at a ratio of 1 g: 13 mL. The mixture was placed in a constant temperature water bath and stirred continuously at 350 r / min for 46 h at 40 °C. After filtration, the mixture was washed with deionized water until no chloride ions were detected in the filtrate with 0.1 mol / L silver nitrate. Then, it was dried at 80 °C and ground to obtain sodium-treated attapulgite.

[0022] A3. The sodium-modified attapulgite obtained in A2 was mixed with hexadecyltrimethylammonium chloride at a mass ratio of 3:1. After sonication for 20 minutes (frequency 40kHz, power 300W), the mixture was transferred to a constant-temperature magnetic stirrer and stirred continuously at 450 r / min for 4.2 hours at 70℃ until the reaction was complete. The resulting mixture was cooled to room temperature, filtered, and washed multiple times with deionized water until no chloride ions were detectable in the filtrate (each time, a small amount of filtrate was acidified with dilute nitric acid and AgNO3 solution was added dropwise to confirm the absence of chloride ions). - (until present), and finally dried at 80℃ for 12 hours, and then ground through a 200-mesh sieve to obtain hexadecyltrimethylammonium chloride modified attapulgite.

[0023] (II) The preparation method of calcified humic acid is as follows: B1. After pulverizing the humic acid, place it in a muffle furnace for calcination. Specifically, heat the calcination temperature to 380℃ at a heating rate of 5℃ / min and calcinate for 1.1h. After stopping the heating, allow it to cool naturally to room temperature and remove it to obtain calcined powder.

[0024] B2, with a solid-liquid ratio of 1:5 (w / v), was soaked in a 2 mol / L calcium chloride solution for 2.2 h with a shaking frequency of 120 rpm. After soaking, the liquid was separated by Buchner funnel filtration, transforming it into insoluble calcium humic acid. B2, with a solid-liquid ratio of 1:4 (w / v), was soaked in a 1 mol / L sodium nitrate solution for 6.8 min, followed by rapid filtration to discard the mother liquor. After washing with water and filtration (repeated with distilled water soaking and filtration 5 times), the sample was spread flat on a tray and placed in an oven at 60℃ for 24 h to avoid structural collapse due to high temperature, thus obtaining calcified humic acid with excellent adsorption capacity.

[0025] (III) A method for preparing an organic compound fertilizer, comprising the following steps: S1. Sun-drying corn stalks and chicken manure separately and crushing them to a particle size of 40 mesh to obtain stalk pellets and chicken manure pellets respectively; specifically, corn stalks are cut into small sections and laid flat in a sunny and ventilated place to dry for 5 days, turning them over 4 times during this period to prevent mold; when the moisture content drops below 15%, they are fed into a hammer mill and crushed to a particle size of 40 mesh to obtain stalk pellets. After collecting chicken manure, removing feathers, stones and other foreign objects, it is also spread out to dry until the moisture content is below 30%, and then fed into a hammer mill and crushed to a particle size of 40 mesh to obtain chicken manure pellets.

[0026] S2. By weight, mix 19 parts straw pellets, 78 parts chicken manure pellets, 22 parts sawdust, 2.7 parts fermentation agent, 3.5 parts hexadecyltrimethylammonium chloride modified attapulgite, and 3.2 parts calcified humic acid evenly. Specifically, first put the dry powders (straw pellets, chicken manure pellets, sawdust, hexadecyltrimethylammonium chloride modified attapulgite, and calcified humic acid) into a horizontal ribbon mixer, run for 3 minutes, then add the fermentation agent, and continue running for 5 minutes to mix the whole mixture.

[0027] S3. Place the mixture into a fermentation tank, pile it to a height of 1.2m to ensure aeration, and ferment it. Turn the pile once a day for 27 days. Specifically, in the early stage of fermentation (days 1-7): maintain the temperature at 55-65℃ (thermophilic stage) and turn the pile once a day; in the middle stage of fermentation (days 8-20): lower the temperature to 40-50℃ (mesothermic stage) and turn the pile every other day; in the late stage of fermentation (days 21-27): bring it to room temperature and turn it once a week; maintain the moisture content at 50-60% throughout the process, and spray water if necessary; after fermentation, dry the material and spread it out in a cool, ventilated place to air dry. Do not expose it to direct sunlight to avoid loss of beneficial components, and you will get the base fertilizer; add 2% of its mass of mineral-derived potassium humate, 0.5% of sodium humate, 0.5% of potassium humate and 2% of polyglutamic acid to the base fertilizer, mix well, and you will get the organic compound fertilizer.

[0028] The fermentation agent is an organic fertilizer fermentation agent, purchased from Guangzhou Weiyuan Biotechnology Co., Ltd.; the fermentation agent includes Bacillus subtilis, Trichoderma harzianum, Bacillus licheniformis, Aspergillus oryzae, and yeast.

[0029] Example 2: The difference between this example and Example 1 is that: a method for preparing an organic compound fertilizer includes the following steps: S1, drying corn stalks and chicken manure in the sun and crushing them to a particle size of 40 mesh to obtain straw pellets and chicken manure pellets respectively.

[0030] S2. By weight, mix 18 parts of straw pellets, 77 parts of chicken manure pellets, 20 parts of sawdust, 2.5 parts of fermentation agent, 3.2 parts of cetyltrimethylammonium chloride-modified attapulgite, and 3 parts of calcified humic acid evenly to obtain a mixture.

[0031] S3. Place the mixture into a fermentation tank and ferment for 27 days. Then discharge and dry the mixture to obtain the base fertilizer. Add 2% by weight of mineral-derived potassium humate, 0.5% by weight of sodium humate, 0.5% by weight of potassium humate and 2% by weight of polyglutamic acid to the base fertilizer and mix well to obtain organic compound fertilizer.

[0032] Example 3: The difference between this example and Example 1 is that: a method for preparing an organic compound fertilizer includes the following steps: S1, drying corn stalks and chicken manure in the sun and crushing them to a particle size of 40 mesh to obtain straw pellets and chicken manure pellets respectively.

[0033] S2. By weight, mix 20 parts of straw pellets, 80 parts of chicken manure pellets, 23 parts of sawdust, 3 parts of fermentation agent, 3.7 parts of cetyltrimethylammonium chloride-modified attapulgite, and 3.5 parts of calcified humic acid evenly to obtain a mixture.

[0034] S3. Place the mixture into a fermentation tank and ferment for 27 days. Then discharge and dry the mixture to obtain the base fertilizer. Add 2% by weight of mineral-derived potassium humate, 0.5% by weight of sodium humate, 0.5% by weight of potassium humate and 2% by weight of polyglutamic acid to the base fertilizer and mix well to obtain organic compound fertilizer.

[0035] Comparative Example 1: The difference between this comparative example and Example 1 is that no cetyltrimethylammonium chloride-modified attapulgite and calcified humic acid are added in the preparation of the organic compound fertilizer.

[0036] Comparative Example 2: The difference between this comparative example and Example 1 is that no calcified humic acid is added in the preparation of the organic compound fertilizer.

[0037] Comparative Example 3: The difference between this comparative example and Example 1 is that no hexadecyltrimethylammonium chloride modified attapulgite is added in the preparation of the organic compound fertilizer.

[0038] Experimental Example: Experimental Subjects: Organic compound fertilizers prepared in Examples 1-3 and Comparative Examples 1-3. Experimental Items: ① Organic matter (%) - determined according to NY / T 525-2021 method; ② Seed germination rate (%) - organic compound fertilizer and water were mixed at a mass ratio of 1:10 and extracted, and 10 mL of the extract was used to culture cucumber seeds. Experimental Results: See Table 1.

[0039] Table 1. Experimental Data

[0040] Results Analysis: Analysis of Examples 1-3 and the data in Table 1 and Figure 1 shows that the organic matter content of the organic compound fertilizer prepared by the present invention (Examples 1-3) reaches more than 54.3%, and the seed germination rate is as high as 91.1%.

[0041] Based on the data in Table 1 and Figure 1, the analysis of Example 1 and Comparative Examples 1-3 is as follows: Specifically, comparing Comparative Examples 1 and 2, it can be seen that, compared to Comparative Example 1, Comparative Example 2, by simply introducing hexadecyltrimethylammonium chloride to modify attapulgite, resulted in a slight decrease in the organic matter content of the prepared organic compound fertilizer, with no significant change. However, the seed germination rate decreased from 85.8% (Comparative Example 1) to 82.3% (Comparative Example 2). This indicates that simply introducing hexadecyltrimethylammonium chloride to modify attapulgite actually leads to a decrease in the seed germination rate of the prepared organic compound fertilizer.

[0042] This is mainly because when hexadecyltrimethylammonium chloride is introduced alone to modify attapulgite, the long-chain alkyl group of hexadecyltrimethylammonium chloride forms a hydrophobic layer on the surface of attapulgite, which blocks the microporous structure, reduces the oxygen permeability of the pile, inhibits the activity of aerobic microorganisms, increases the residual organic acids / aldehydes, and has a negative impact, resulting in a decrease in seed germination rate.

[0043] Specifically, comparing Comparative Example 1 and Comparative Example 3, it can be seen that compared to Comparative Example 1, the addition of calcified humic acid alone in Comparative Example 3 resulted in a slight decrease in the organic matter content of the prepared organic compound fertilizer, with no significant change. However, the seed germination rate increased from 85.8% (Comparative Example 1) to 88.7% (Comparative Example 3), indicating that the addition of calcified humic acid alone can improve the seed germination rate of the prepared organic compound fertilizer.

[0044] In comparison with Example 1, it can be seen that the simultaneous introduction of hexadecyltrimethylammonium chloride to modify attapulgite and calcified humic acid can produce a synergistic effect, which can synergistically improve the seed germination rate test data of the prepared organic compound fertilizer.

[0045] This is mainly because, when both calcified humic acid and hexadecyltrimethylammonium chloride are introduced to modify attapulgite, on the one hand, the calcified humic acid and hexadecyltrimethylammonium chloride-modified attapulgite form a composite structure through calcium bridges, which is beneficial for increasing oxygen transport efficiency and promoting the proliferation of aerobic bacteria, effectively weakening / counteracting the negative effects of introducing hexadecyltrimethylammonium chloride-modified attapulgite alone. On the other hand, in the early stage, hexadecyltrimethylammonium chloride-modified attapulgite rapidly adsorbs free ammonium, avoiding early ammonia volatilization; in the middle stage, calcified humic acid slowly releases Ca... 2+ Activates urease, promoting the adsorption of NH4 + Directed conversion to NO3 -Later, as the nitrifying bacteria community matures, nitrogen utilization significantly improves, thus achieving a synergistic effect of increasing seed germination rate.

[0046] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

[0047] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.

Claims

1. A method for preparing an organic compound fertilizer, characterized in that, Includes the following steps: S1. Sun-dry and crush corn stalks and chicken manure to obtain stalk pellets and chicken manure pellets; S2. Mix 18-20 parts by weight of the stalk pellets, 77-80 parts by weight of chicken manure pellets, 20-23 parts by weight of sawdust, 2.5-3 parts by weight of fermentation agent, 3.2-3.7 parts by weight of cetyltrimethylammonium chloride-modified attapulgite, and 3-3.5 parts by weight of calcified humic acid to obtain a mixture; S3. Place the mixture in a fermentation tank, ferment for 25-28 days, discharge, dry, and obtain base fertilizer; add 2.8-3.2% by weight of humic acid and 1.8-2.1% by weight of polyglutamic acid, mix well, and obtain the organic compound fertilizer.

2. The method for preparing organic compound fertilizer according to claim 1, characterized in that, The preparation method of the hexadecyltrimethylammonium chloride modified attapulgite is as follows: A1. Attapulgite is treated with hydrochloric acid solution, filtered, washed, and dried to obtain pretreated attapulgite; A2. The pretreated attapulgite obtained in A1 is treated with sodium chloride solution, filtered, washed, and dried to obtain sodium-modified attapulgite; A3. The sodium-modified attapulgite obtained in A2 is mixed with hexadecyltrimethylammonium chloride at a mass ratio of 3:1, ultrasonicated, stirred at 70±5℃ for 4-4.5h, cooled to room temperature, filtered, washed, and dried to obtain the final product.

3. The method for preparing organic compound fertilizer according to claim 2, characterized in that, The specific operation of A1 is as follows: Mix attapulgite with hydrochloric acid solution with a concentration of 1±0.1mol / L at a ratio of 1g:(3.5-4.5)mL and stir. After stirring for 120-150min, take the suspension, filter, wash until neutral, dry, and crush to obtain pretreated attapulgite.

4. The method for preparing organic compound fertilizer according to claim 2, characterized in that, The specific operation of A2 is as follows: the pretreated attapulgite obtained from A1 is mixed with a sodium chloride solution with a concentration of 1±0.1mol / L at a ratio of 1g:(12-14)mL, stirred at 40±2℃ for 45-48h, filtered, washed with water, dried, and ground to obtain sodium-treated attapulgite.

5. The method for preparing organic compound fertilizer according to claim 1, characterized in that, The preparation method of the calcified humic acid is as follows: B1. After crushing the humic acid, calcining it and cooling it to obtain calcined powder; B2. First soaking the calcined powder obtained in B1 in calcium chloride solution for 2-2.5h, then filtering it; then soaking it in sodium nitrate solution for 5-8min, then filtering it; washing it with water and filtering it again, then drying it, the calcined humic acid is obtained.

6. The method for preparing organic compound fertilizer according to claim 5, characterized in that, In B1, the calcination temperature is 370-400℃ and the calcination time is 1-1.2h.

7. The method for preparing organic compound fertilizer according to claim 5, characterized in that, In B2, the concentration of the calcium chloride solution is 2 ± 0.1 mol / L; the concentration of the sodium nitrate solution is 1 ± 0.1 mol / L.

8. The method for preparing organic compound fertilizer according to claim 1, characterized in that, In S1, the particle size of the straw pellets and chicken manure pellets does not exceed 40 mesh.

9. The method for preparing organic compound fertilizer according to claim 1, characterized in that, In S2, the fermentation agent includes Bacillus subtilis, Bacillus licheniformis, Trichoderma harzianum, Aspergillus oryzae, and Rhodotorula rubra.

10. An organic compound fertilizer, characterized in that, It is prepared by the preparation method described in any one of claims 1 to 9.

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