CN114292145A - Preparation method of artificial humic acid urea slow-release fertilizer - Google Patents
Preparation method of artificial humic acid urea slow-release fertilizer Download PDFInfo
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Abstract
A preparation method of artificial humic acid urea slow release fertilizer relates to a preparation method of slow release fertilizer. The invention aims to solve the problems that the existing preparation method of the humic acid urea fertilizer is high in cost, unstable in product quality, excessive in heavy metal and the influence on soil and environment caused by the large loss of nitrogen fertilizer in agriculture is caused. The method comprises the following steps: firstly, preparing a solid-liquid mixed product containing artificial humus; secondly, preparing artificial humic acid powder; and thirdly, mixing the artificial humic acid powder with the urea solution, reacting, and freeze-drying to obtain the artificial humic acid urea slow-release fertilizer. According to the invention, the artificial humic acid urea slow-release fertilizer is synthesized by reacting humic acid and urea prepared from agricultural solid waste biomass, so that the nitrogen content in the artificial humic acid urea is improved, the long-acting slow-release effect of the urea fertilizer is further improved, the heavy metal and impurity content in the urea fertilizer can be reduced, and the use effect is improved. The invention can obtain the artificial humic acid urea slow release fertilizer.
Description
Technical Field
The invention relates to a preparation method of a slow-release fertilizer.
Background
The synthetic technology of the artificial humic acid urea fertilizer plays an important role in the resource utilization of industrial and agricultural organic wastes. By applying the artificial humic acid technology and the corresponding innovative fertilizer processing technology, a fertilizer product integrating green, high-energy and high-efficiency can be produced, the development of the green and environment-friendly fertilizer industry can be powerfully promoted, and the requirements of modern agriculture and environmental protection industry in China are met. The humic acid urea can prolong the retention time of nitrogen elements in the urea in soil, prolong the fertilizer efficiency and play a role in slow release, so the humic acid urea is widely applied to the long-acting slow release urea. The existing humic acid long-acting slow-release urea is produced by activating mineral sources (minerals such as lignite, leonardite, sewage sludge and the like) to obtain mineral source humic acid (the content of the common humic acid is 40-50%), and then carrying out complexing reaction granulation or spraying and coating on the mineral source humic acid and urea. At present, the humic acid urea fertilizer is prepared by methods such as a mechanical mixing method, a solvent method, a melting process and the like in the research, wherein the melting process is more convenient for production and operation on the basis of most complete contact of reactants. The humic acid-urea compound fertilizer is generally produced by a humic acid wrapping method and a simple blending granulation method, which strictly speaking does not belong to the definition of humic acid-urea, because the humic acid and the urea produced by the technology basically do not have chemical complexation reaction, acid-base neutralization reaction, carbonyl nucleophilic addition reaction and free radical reaction. The coating and coating effects of humic acid and urea are realized only by a physical method, and the following reasons mainly exist: the mineral source humic acid and urea are subjected to complex reaction to generate the mineral source humic acid urea, and the water solubility of the mineral source humic acid urea is low; due to the difference of the source and the production and processing technology of the mineral humic acid, the content of the components in the mineral humic acid is greatly different, and the mineral humic acid not only has one component of the humic acid, but also possibly contains fulvic acid and other heavy metal components. Mineral sources (mineral substances such as lignite, weathered lignite, sewage sludge and the like) are used as raw materials, the contents of heavy metals such as lead, mercury, copper and the like in humic acid subjected to activation treatment by substances such as alkali and the like are always in an excessive level, the humic acid serving as a fertilizer is used for a long time, the heavy metal accumulation in soil and the excessive heavy metal content in crops are seriously influenced, and high-quality agricultural products are difficult to produce. However, there is no technology or method for removing or eliminating heavy metal components in humic acid of mineral origin. Humic acid is extracted from agricultural solid waste biomass, so that agricultural solid waste resources are better recycled, and an important role is played in plant growth regulation. Excessive and improper application of nitrogen fertilizer can cause a number of problems in agricultural soils, such as inefficient nitrogen use, environmental pollution, and human health risks. Urea is widely used as a nitrogen source in many crop production systems because of its high nitrogen content. However, the nitrogen recovery of urea in soil plant systems rarely exceeds 50% of nitrogen application. The main reasons for low nitrogen utilization are leaching, denitrification and volatilization. Therefore, there is a need to prepare a high-efficiency, green, slow-release, non-polluting urea fertilizer to alleviate agricultural and environmental requirements.
Disclosure of Invention
The invention aims to solve the problems that the existing preparation method of the urea humate fertilizer is high in cost, unstable in product quality, excessive in heavy metal and the influence on soil and environment caused by the large loss of nitrogen fertilizer in agriculture, and provides the preparation method of the artificial urea humate slow-release fertilizer.
A preparation method of artificial humic acid urea slow release fertilizer comprises the following steps:
firstly, mixing biomass powder, an active additive and water, then putting the mixture into a reaction kettle, controlling a temperature rise program of the reaction kettle, carrying out hydrothermal humification reaction on the biomass powder under the conditions of high temperature and high pressure, and then cooling the mixture to room temperature to obtain a solid-liquid mixed product containing artificial humus;
secondly, carrying out suction filtration on the solid-liquid mixed product containing the artificial humus, and removing solids to obtain artificial humus liquid; adjusting the pH value of the artificial humus liquid to 1, and standing to obtain a solid substance; taking deionized water as a cleaning agent, performing centrifugal cleaning on the solid matter for multiple times until the solid matter is neutral, performing vacuum drying to obtain artificial humic acid solid, and crushing to obtain artificial humic acid powder;
thirdly, mixing urea with water, and putting the mixture into an oven for pyrolysis to obtain a urea solution;
secondly, mixing the artificial humic acid powder with the urea solution, putting the mixture into an oven for reaction, and cooling the mixture to room temperature to obtain a precursor of the artificial humic acid urea solid;
and thirdly, freeze-drying the precursor of the urea artificial humic acid solid, and then crushing to obtain the urea artificial humic acid slow-release fertilizer.
The invention has the beneficial effects that:
1. the artificial humic acid urea slow-release fertilizer prepared by the invention adopts the least amount of added urea to obtain higher nitrogen content and meet the requirements of agricultural production;
2. according to the invention, the agricultural solid waste organisms are subjected to hydrothermal humification treatment, the solid waste organisms are reused to produce artificial humic acid, a green soil conditioner with the same efficacy as mineral humic acid is obtained, and the artificial humic acid urea slow-release fertilizer is fused with urea to obtain the efficient and green artificial humic acid urea slow-release fertilizer;
3. the invention prepares the artificial humic acid urea by a melt infiltration method, so that the urea and the artificial humic acid fully react and fully contact with each other to obtain a stronger water-soluble artificial humic acid urea fertilizer;
4. according to the artificial humic acid urea slow-release fertilizer prepared by the invention, the green soil additive artificial humic acid and urea meeting the growth of crops are subjected to chemical reaction combination to obtain the artificial humic acid urea slow-release fertilizer with higher nitrogen content and stronger water solubility;
5. the agricultural solid waste biomass is wide in material source, low in price and easy to obtain, and the manufacturing cost of the artificial humic acid urea slow-release fertilizer is reduced; the operation is simple, green, environment-friendly and pollution-free, and the method is beneficial to wide application in actual production;
6. the artificial humic acid urea slow-release fertilizer prepared by the invention is synthesized by reacting humic acid prepared from agricultural solid waste biomass with urea, so that the nitrogen content in the artificial humic acid urea is improved, the long-acting slow-release effect of the urea fertilizer is improved, the heavy metal and impurity content in the urea fertilizer can be reduced, and the use effect is improved.
The invention can obtain the artificial humic acid urea slow release fertilizer.
Drawings
FIG. 1 is a scanning electron micrograph of an artificial humic acid solid obtained in step two of example 1;
FIG. 2 is a scanning electron micrograph of the humic acid-urea slow release fertilizer obtained in example 1;
FIG. 3 is a FTIR profile of the artificial urea humate slow release fertilizer prepared in example 1; in the figure, 1 is an FTIR curve of the artificial humic acid solid obtained in the second step of the example 1, and 2 is an FTIR curve of the artificial humic acid urea slow release fertilizer prepared in the example 1;
FIG. 4 is an XRD pattern of the artificial urea humate slow release fertilizer prepared in example 1; in the figure, 1 is an XRD curve of the artificial humic acid solid obtained in the second step of example 1, and 2 is an XRD curve of the artificial humic acid urea slow release fertilizer prepared in example 1;
FIG. 5 shows the slow release fertilizer of artificial humic acid urea prepared in example 113C NMR chart.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the artificial humic acid urea slow-release fertilizer of the embodiment is completed according to the following steps:
firstly, mixing biomass powder, an active additive and water, then putting the mixture into a reaction kettle, controlling a temperature rise program of the reaction kettle, carrying out hydrothermal humification reaction on the biomass powder under the conditions of high temperature and high pressure, and then cooling the mixture to room temperature to obtain a solid-liquid mixed product containing artificial humus;
secondly, carrying out suction filtration on the solid-liquid mixed product containing the artificial humus, and removing solids to obtain artificial humus liquid; adjusting the pH value of the artificial humus liquid to 1, and standing to obtain a solid substance; taking deionized water as a cleaning agent, performing centrifugal cleaning on the solid matter for multiple times until the solid matter is neutral, performing vacuum drying to obtain artificial humic acid solid, and crushing to obtain artificial humic acid powder;
thirdly, mixing urea with water, and putting the mixture into an oven for pyrolysis to obtain a urea solution;
secondly, mixing the artificial humic acid powder with the urea solution, putting the mixture into an oven for reaction, and cooling the mixture to room temperature to obtain a precursor of the artificial humic acid urea solid;
and thirdly, freeze-drying the precursor of the urea artificial humic acid solid, and then crushing to obtain the urea artificial humic acid slow-release fertilizer.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the biomass powder in the step one is one or a mixture of more of rice straw, corn straw, soybean straw, leaves and sawdust, and the particle size of the biomass powder is 50-100 meshes. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the active auxiliary agent in the step one is NaOH, KOH, industrial soda ash and Ca (OH)2、Ca(OH)2With Na2CO3One or a mixture of several of them. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the mass ratio of the biomass powder, the active assistant and the water in the step one is (3-5): (0.1-2): 25-100). The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the temperature of the hydrothermal humification reaction in the step one is 180-200 ℃, the pressure is 0.5-5 MPa, and the time is 20-28 h. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: and the standing time in the step two is 5-8 h. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: in the second step, the rotating speed of each centrifugal cleaning is 5000r/min to 8000r/min, and the centrifugal cleaning time is 3min to 5 min; the temperature of the vacuum drying in the second step is 50-60 ℃. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the volume ratio of the mass of the urea to the water in the third step is 1.1: 1; and the pyrolysis temperature in the third step is 40 ℃, and the pyrolysis time is 0.1-0.3 h. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the mass ratio of the artificial humic acid powder in the third step to the urea in the third step is 1: 3; the reaction temperature in the third step is 130 ℃, and the reaction time is 1-1.5 h. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: and thirdly, the temperature of the freeze drying in the third step is-80 ℃ and the time is 20-24 h. The other steps are the same as those in the first to ninth embodiments.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1: a preparation method of artificial humic acid urea slow release fertilizer comprises the following steps:
firstly, washing eucalyptus leaves for 5 times, then drying at 60 ℃, and grinding into powder with the particle size of 0.1-1 mm by using powder grinding to obtain leaf powder; mixing the leaf powder, the active additive and water, then putting the mixture into a reaction kettle, controlling the temperature rise program of the reaction kettle, carrying out hydrothermal humification reaction on the leaf powder under the conditions of high temperature and high pressure, and then cooling the mixture to room temperature to obtain a solid-liquid mixed product containing artificial humus;
the mass ratio of the leaf powder, the active additive and the water in the step one is 4:1: 100;
the active auxiliary agent in the step one is KOH;
the temperature of the hydrothermal humification reaction in the step one is 200 ℃, the pressure is 2.0MPa, and the time is 24 h;
secondly, carrying out suction filtration on the solid-liquid mixed product containing the artificial humus, and removing solids to obtain artificial humus liquid; regulating the pH value of the artificial humus liquid to 1 by using hydrochloric acid with the concentration of 6mol/L, and standing for 5 hours to obtain a solid substance; taking deionized water as a cleaning agent, performing centrifugal cleaning on the solid matter for multiple times until the solid matter is neutral, performing vacuum drying at 50 ℃ to obtain artificial humic acid solid, and crushing to obtain artificial humic acid powder;
the rotating speed of the centrifugal cleaning in the step two is 8000r/min, and the time of the centrifugal cleaning is 3 min;
thirdly, mixing urea with ultrapure water, and putting the mixture into an oven for pyrolysis to obtain a urea solution;
the volume ratio of the mass of the urea to the ultrapure water in the third step is 1.1: 1;
the pyrolysis temperature in the third step is 40 ℃, and the pyrolysis time is 0.2 h;
secondly, mixing the artificial humic acid powder with the urea solution, putting the mixture into an oven for reaction, and cooling the mixture to room temperature to obtain a precursor of the artificial humic acid urea solid;
the mass ratio of the artificial humic acid powder in the third step to the urea in the third step is 1: 3;
the reaction temperature in the third step is 130 ℃, and the reaction time is 1.3 h;
thirdly, freeze-drying the precursor of the urea solid of artificial humic acid, and then crushing to obtain the urea slow-release fertilizer of artificial humic acid;
and thirdly, the temperature of the freeze drying in the third step is-80 ℃, and the time is 24 hours.
The artificial urea humate slow-release fertilizer prepared in the embodiment 1 can obtain the maximum nitrogen content by adopting the minimum urea addition amount, the nitrogen content of the artificial urea humate slow-release fertilizer can reach more than 36.20%, and the content of artificial humic acid is 44.09%.
FIG. 1 is a scanning electron micrograph of an artificial humic acid solid obtained in step two of example 1;
as can be seen from the scanning electron microscope image, the artificial humic acid solid is mutually agglomerated to form a blocky substance with larger particles, and the properties are not uniform.
FIG. 2 is a scanning electron micrograph of the humic acid-urea slow release fertilizer obtained in example 1;
as can be seen from the scanning electron microscope picture, the electron microscope picture of the artificial humic acid urea slow release fertilizer is granular, and during infiltration, urea nitrogen or other forms of nitrogen, such as NH4 +-N，NH3N, which is uniformly loaded on the surface and in the structure of the humic acid.
FIG. 3 is a FTIR profile of the artificial urea humate slow release fertilizer prepared in example 1; in the figure, 1 is an FTIR curve of the artificial humic acid solid obtained in the second step of the example 1, and 2 is an FTIR curve of the artificial humic acid urea slow release fertilizer prepared in the example 1;
the slow release fertilizer of artificial humic acid urea is 3500-3300cm-1In the presence of a strong amide (NH)2) Antisymmetric telescopic peaks. The double peak may be the generation of primary amine during the fusion of artificial humic acid and urea, and the primary amine has a single peak between 1650-1570. At 1680cm-1And 1600cm-1Peaks appeared due to C ═ O double bond stretching vibration and primary amine NH in-plane stretching vibration of the amide, respectively. At 1159cm-1The vibrational peak at the spectrum is represented by C-N stretching vibration of the secondary amine. Compared with the artificial humic acid, the slow release fertilizer of the artificial humic acid urea has two broad peaks near 3445 and 3214, which can be basically determined to be-OH of the artificial humic acid and-NH of the urea2Hydrogen bonds or complex bonds are formed.
FIG. 4 is an XRD pattern of the artificial urea humate slow release fertilizer prepared in example 1; in the figure, 1 is an XRD curve of the artificial humic acid solid obtained in the second step of example 1, and 2 is an XRD curve of the artificial humic acid urea slow release fertilizer prepared in example 1;
as Urea or Urea-N is loaded to the artificial humic acid, the artificial humic acid Urea slow release fertilizer has higher degree of crystallization order.
FIG. 5 shows the slow release fertilizer of artificial humic acid urea prepared in example 113C NMR chart.
Example 1 preparation of humanMethod for preparing industrial humic acid urea slow release fertilizer13The C NMR chart (shown in figure 5) shows that the content of aliphatic carbon and aromatic carbon in the artificial humic acid urea slow release fertilizer is high.
Example 2: an indoor pot experiment is adopted to verify the effect of the artificial humic acid urea slow-release fertilizer. Culture test soil to be tested is surface soil of 0-20cm collected from a test field of northeast agriculture university, and the surface soil is ground and sieved by a 2mm sieve after being naturally air-dried. The experiment designed a total of three treatments, three replicates of each treatment. Respectively as follows: a control (CK, without any fertilizer added), normal urea (U) and the artificial urea humate slow-release fertilizer (A-HAU) prepared in example 1 were set, and the nitrogen fertilizer application rate was 200mg/kg dry soil. The specific operation is as follows: weighing an air-dried soil sample (passing through a 1mm sieve) equivalent to 100g of dry soil, placing the air-dried soil sample in a flowerpot, adjusting the water content of the soil to 40% of the maximum water holding capacity in the field, and pre-culturing the soil sample at 25 ℃ for four days to activate the microbial activity of the soil and reduce the change of the microbial activity of the soil caused by adding water into the dry soil in the initial culture stage. To ensure that the fertilizer content in the sampled soil was as consistent as possible, all fertilizers were added to the soil as aqueous solutions, the pH of the solutions was adjusted to 7 (the pH of the solutions was adjusted with 0.5M NaOH and 1M HCl), and the mixture was stirred well. After the pre-incubation was completed, the soil moisture content of all samples was maintained at 60% of the soil moisture content. In order to ensure constant soil moisture during the whole test period, the moisture is supplemented by a weighing method every 4 days. All 63 pots of the three treatments were cultured in a light incubator and destructive sampling was performed on days 0,1,3,7,14,28, and 70 to determine changes in total nitrogen content in the soil.
Table 1 shows the trend of total nitrogen (%) in the artificial urea humate fertilizer prepared in example 1 and other treatments.
TABLE 1
As can be seen from Table 1, the artificial urea humate slow-release fertilizer prepared in example 1 has a significant slow-release effect on soil. Compared with CK, the nitrogen content is higher than that of CK at different stages. Compared with U, the nitrogen content of the artificial humic acid urea slow-release fertilizer is higher than that of U after 14 days. The nitrogen content is in a reduced state in the first fourteen days, which shows that the artificial humic acid urea slow-release fertilizer is easier to be decomposed and utilized by soil microorganisms. After 14 days, the nitrogen content of the artificial humic acid urea slow release fertilizer is increased, which indicates that the artificial humic acid urea slow release fertilizer can fix nitrogen more effectively and achieve the slow release effect.
Table 2 shows the pH trend change of the artificial urea humate fertilizer prepared in example 1 and other treatments;
TABLE 2
As can be seen from the table, the artificial urea humate slow-release fertilizer prepared in example 1 lowered the pH of the soil, while CK and U hardly changed the pH of the soil.
Example 3: an indoor pot experiment is adopted to verify the influence of the artificial humic acid urea slow release fertilizer on plants. Culture test soil to be tested is surface soil of 0-20cm collected from a test field of northeast agriculture university, and the surface soil is ground and sieved by a 2mm sieve after being naturally air-dried. The experiment designed a total of three treatments, four replicates each. Respectively as follows: a control (CK, without any fertilizer added), normal urea (U) and the artificial urea humate slow-release fertilizer (A-HAU) prepared in example 1 were set, and the nitrogen fertilizer application rate was 200mg/kg dry soil. The specific operation is as follows: weighing an air-dried soil sample (passing through a 1mm sieve) equivalent to 500g of dry soil, placing the air-dried soil sample in a flowerpot, adjusting the water content of the soil to 40% of the maximum water holding capacity in the field, and pre-culturing the soil sample at 25 ℃ for four days to activate the microbial activity of the soil and reduce the change of the microbial activity of the soil caused by adding water into the dry soil in the initial culture stage. In order to ensure that the fertilizer in the soil is absorbed and utilized by the plants to the maximum extent, all the fertilizer is added into the soil in the form of aqueous solution, the pH value of the solution is adjusted to 7 (the pH value of the solution is adjusted by 0.5M NaOH and 1M HCl), and the mixture is stirred uniformly. After the preculture was completed, four corn seeds with consistent germination were sown in each pot (the seeds were sterilized with 1% sodium hypochlorite for 30 minutes, rinsed 5 times with ultrapure water, and germinated in the dark). Only 2 plants with the same growth vigor are left in each flowerpot after one week. All soil moisture contents treated were maintained at 60% of the soil moisture capacity. In order to ensure constant soil moisture during the whole test period, a weighing method is adopted to supplement moisture every day. Until the end of the culture on day 60.
Table 3 shows the growth trend change table of the artificial urea humate fertilizer prepared in example 1 and other treated plants;
TABLE 3
As can be seen from the table, the artificial humic acid urea slow release fertilizer prepared in example 1 promotes various physiological indexes of plants, and particularly, compared with a control, the artificial humic acid urea slow release fertilizer is remarkably promoted. Compared with the method of applying urea, the artificial humic acid urea slow release fertilizer still promotes various physiological indexes of plants, but the promotion effect is not obvious. The artificial humic acid urea slow release fertilizer can promote the growth of plants like urea, and solves the major problem of nitrogen fertilizer shortage in the world.
Claims (10)
1. A preparation method of artificial urea humate slow-release fertilizer is characterized in that the preparation method of the artificial urea humate slow-release fertilizer is completed according to the following steps:
firstly, mixing biomass powder, an active additive and water, then putting the mixture into a reaction kettle, controlling a temperature rise program of the reaction kettle, carrying out hydrothermal humification reaction on the biomass powder under the conditions of high temperature and high pressure, and then cooling the mixture to room temperature to obtain a solid-liquid mixed product containing artificial humus;
secondly, carrying out suction filtration on the solid-liquid mixed product containing the artificial humus, and removing solids to obtain artificial humus liquid; adjusting the pH value of the artificial humus liquid to 1, and standing to obtain a solid substance; taking deionized water as a cleaning agent, performing centrifugal cleaning on the solid matter for multiple times until the solid matter is neutral, performing vacuum drying to obtain artificial humic acid solid, and crushing to obtain artificial humic acid powder;
thirdly, mixing urea with water, and putting the mixture into an oven for pyrolysis to obtain a urea solution;
secondly, mixing the artificial humic acid powder with the urea solution, putting the mixture into an oven for reaction, and cooling the mixture to room temperature to obtain a precursor of the artificial humic acid urea solid;
and thirdly, freeze-drying the precursor of the urea artificial humic acid solid, and then crushing to obtain the urea artificial humic acid slow-release fertilizer.
2. The preparation method of the artificial humic acid urea slow release fertilizer as claimed in claim 1, wherein the biomass powder in the first step is one or a mixture of more of rice straw, corn straw, soybean straw, leaves and wood chips, and the particle size of the biomass powder is 50-100 meshes.
3. The method for preparing artificial humic acid and urea slow release fertilizer as claimed in claim 1, wherein said active auxiliary agent in step one is NaOH, KOH, industrial soda ash and Ca (OH)2、Ca(OH)2With Na2CO3One or a mixture of several of them.
4. The method for preparing the artificial humic acid and urea slow release fertilizer as claimed in claim 1, wherein the mass ratio of the biomass powder, the active auxiliary agent and the water in the step one is (3-5): (0.1-2): 25-100.
5. The method for preparing the artificial humic acid and urea slow release fertilizer as claimed in claim 1, wherein the temperature of the hydrothermal humification reaction in the first step is 180 ℃ to 200 ℃, the pressure is 0.5MPa to 5MPa, and the time is 20h to 28 h.
6. The method for preparing the artificial humic acid and urea slow release fertilizer as claimed in claim 1, wherein the standing time in the second step is 5-8 h.
7. The method for preparing the artificial humic acid urea slow release fertilizer as claimed in claim 1, wherein the rotation speed of each centrifugal cleaning in the second step is 5000r/min to 8000r/min, and the time of the centrifugal cleaning is 3min to 5 min; the temperature of the vacuum drying in the second step is 50-60 ℃.
8. The method for preparing the artificial humic acid urea slow-release fertilizer as claimed in claim 1, wherein the volume ratio of the mass of the urea to the volume of the water in the third step is 1.1: 1; and the pyrolysis temperature in the third step is 40 ℃, and the pyrolysis time is 0.1-0.3 h.
9. The method for preparing the artificial humic acid urea slow release fertilizer according to claim 1, wherein the mass ratio of the artificial humic acid powder in the third step to the urea in the third step is 1: 3; the reaction temperature in the third step is 130 ℃, and the reaction time is 1-1.5 h.
10. The method for preparing the artificial humic acid and urea slow release fertilizer as claimed in claim 1, wherein the freeze drying temperature in the third step is-80 ℃ for 20-24 hours.
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| CN109516837A (en) * | 2019-01-28 | 2019-03-26 | 黄国华 | Plant source humic acid long-acting slow-release carbamide fertilizer and its production technology |
| CN113563603A (en) * | 2021-07-05 | 2021-10-29 | 清华大学 | Method for strengthening hydrothermal humification of lignocellulose waste by acid hydrothermal pretreatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109516837A (en) * | 2019-01-28 | 2019-03-26 | 黄国华 | Plant source humic acid long-acting slow-release carbamide fertilizer and its production technology |
| CN113563603A (en) * | 2021-07-05 | 2021-10-29 | 清华大学 | Method for strengthening hydrothermal humification of lignocellulose waste by acid hydrothermal pretreatment |
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