CN111234836B - Soil conditioner containing humic acid and preparation method thereof - Google Patents
Soil conditioner containing humic acid and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to soil improvement conditioners and methods. A soil conditioner containing humic acid comprises the following active ingredients in percentage by mass: organic fertilizer, humic acid, CaO and MgO; the pH value of the soil conditioner is 9.0-12.0; the humic acid is sulfonated lignite humic acid. The application of the soil conditioner can increase the yield of rice, and has a good application prospect.
Description
Technical Field
The invention relates to a soil improvement conditioner and a method, in particular to a soil conditioner containing humic acid and a preparation method thereof.
Background
The soil conditioner is also called soil conditioner, and is a material which can improve the physical property of soil and promote the nutrient absorption of crops, but does not provide plant nutrients. The soil amendment utility principle is to bind many small soil particles to form large, water-stable aggregates. The method is widely applied to the aspects of preventing soil from being corroded, reducing water evaporation or excessive transpiration of the soil, saving irrigation water and promoting healthy growth of plants.
Common soil conditioners comprise polysaccharides, alkali silicate, synthetic foam with open pores, humic acid conditioner and applied salt inhibitor, the humic acid conditioner is a great variety at present, humic acid is a complex reticular polymer containing a large amount of different functional groups and a large amount of carbon, hydrogen, oxygen, nitrogen, sulfur and other metal elements.
Humic acid is mainly formed by animal and plant remains in water bodies under the action of geological conditions and microorganisms, and a large amount of humic acid components exist in peat, weathered coal and lignite. Humic acid can improve soil properties, change soil nutrient composition and increase soil biological activity, and is widely applied to fertilizer preparation, desert greening and barren soil improvement. In order to improve the water solubility of the humic acid and further improve the application effect and convenience, the humic acid can be subjected to sulfonation modification, and the used sulfonating agent mainly comprises sulfuric acid, sulfur trioxide, sulfur dioxide, sulfite and the like; the sulfuric acid method has high sulfonation rate and low cost, but has the defects of wastewater treatment and subsequent alkalization processes; the raw materials and equipment components for treating sulfur trioxide and sulfur dioxide are high; the sulfite method has mild reaction conditions but poor sulfonation effect, and is less in application at present.
Disclosure of Invention
In order to solve the technical problems, the application aims to provide a soil conditioner containing humic acid, which can improve the pH value, the cation exchange capacity and the soil base saturation of acid soil, reduce the contents of soil exchangeable aluminum and available magnesium, enhance the soil tiltability and fertilizer retention capacity and be beneficial to the improvement of the acid soil. Particularly, the sulfonated lignite humic acid is added, the sulfonated lignite humic acid has high water solubility and high dispersibility, the water absorption performance of the compound fertilizer is improved, further, the sulfonated lignite humic acid product is used as a main component, and the sulfonated lignite humic acid product is sulfonated by using a small amount of sulfuric acid matched with sulfite, so that the water solubility and the dispersibility are improved.
In order to achieve the above object, the present application adopts the following technical solutions:
a soil conditioner containing humic acid comprises the following active ingredients in percentage by mass:
20.0 to 40.0 percent of organic fertilizer
Humic acid 8.0-25%
CaO 15.0-30.0%
MgO 8.0-20.0%
The pH value of the soil conditioner is 9.0-12.0; the humic acid is sulfonated lignite humic acid which is prepared by sulfonating lignite humic acid. The pH value of the soil conditioner is measured by a soil pH value measuring method.
Preferably, the soil conditioner comprises the following active ingredients in percentage by mass:
25.0 to 35.0 percent of organic fertilizer
Humic acid 10.0-20%
CaO 15.0-25.0%
MgO 10.0-15.0%
The pH value of the soil conditioner is 9.0-12.0; the humic acid is sulfonated lignite humic acid which is prepared by sulfonating lignite humic acid.
As a further improvement, the preparation method of the sulfonated lignite humic acid product comprises the following steps:
(1) crushing lignite into fine particles by using a crusher;
(2) optionally, adding the fine particles into an oxidant solution for oxidation;
(3) adding the obtained mixture/fine particles into NaOH aqueous solution, and stirring;
(4) centrifuging to remove solids, filtering, and adding concentrated HCI into the obtained filtrate with stirring to adjust pH until a large amount of black precipitate is separated out;
(5) filtering and drying the precipitated precipitate to obtain lignite humic acid;
(6) dissolving humic acid of lignite in water, adding H2SO4And/or K2SO3Reacting;
(7) and drying the solution to obtain a sulfonated lignite humic acid product.
Wherein in the step (2), the fine particles are added to a 20% H2O2 solution in an amount of 0.6 times the mass thereof, and stirred at 50 ℃ for 30 minutes.
Further, in the step (3), the mixture was added to 1.5 times by mass of a 1.5% aqueous solution of KOH, and the stirring was continued at 60 ℃ for 30 minutes.
Further, in the step (6), the lignite humic acid is dissolved in water with the mass being 10 times that of the lignite humic acid, and the reaction is carried out for 2 hours at the temperature of 50 ℃.
Further, 0.5% by mass of H was used in the step (6)2SO4And/or 4% by mass of K2SO3。
Further, 0.5% by mass of H was used in the step (6)2SO4And 4% by mass of K2SO3。
Further, organic fertilizer is used for fermenting one or more of chicken manure, fermented straw and wormcast.
In another aspect, the present application also provides a method for preparing a humic acid-containing soil conditioner, comprising the steps of:
(1) crushing lignite into fine particles by using a crusher;
(2) optionally, adding the fine particles into an oxidant solution for oxidation;
(3) adding the obtained mixture/fine particles into NaOH aqueous solution, and stirring;
(4) centrifuging to remove solids, filtering, and adding concentrated HCI into the obtained filtrate with stirring to adjust pH until a large amount of black precipitate is separated out;
(5) filtering and drying the precipitated precipitate to obtain lignite humic acid;
(6) dissolving humic acid of lignite in water, adding H2SO4And/or K2SO3Reacting;
(7) drying the solution to obtain a sulfonated lignite humic acid product;
(8) and (4) grinding the humic acid product of the sulfonated lignite prepared in the step (7), adding an organic fertilizer and a calcium-magnesium fertilizer, uniformly mixing, grinding and micronizing to obtain the humic acid-containing soil conditioner.
The application adopts the mineral source humic substance as a main raw material, prepares the sulfonated lignite humic acid by sulfonating a small amount of sulfuric acid in cooperation with sulfite, the sulfonated lignite humic acid has high water solubility and high dispersibility, and the water absorption performance of the compound fertilizer is improved. Compared with the control treatment without applying the soil conditioner, the application of the soil conditioner can improve the pH value, the cation exchange capacity and the soil base saturation of the acid soil, reduce the content of soil exchangeable aluminum and effective manganese, enhance the soil tiltability and fertilizer retention capacity and be beneficial to the improvement of the acid soil. The application of the soil conditioner can increase the yield of the rice by 20.9-30.2% on average, and has a good application prospect.
Detailed Description
The main raw materials and reagents used in the examples are as follows:
lignite sample: purchased from enterprises under the Jinzao coal group, and the production place is Shanxi Lingqiu (the experimental batch is detected to contain 45.5 percent of total humic acid, 25.4 percent of water and 22.1 percent of fixed carbon);
sulfonating agent K2SO3And H2SO4Produced by the chemical reagent factory of Xian;
surface tension meter: germany Sita SITA t-100 surface tension meter;
the rest reagents and instruments are all conventional domestic models and types
Only a portion of representative results are shown in the examples and a number of methodological/performance-analogous experiments are not shown.
Example 1 basic Performance test method
And (3) measuring the sulfonation degree:
weighing by an analytical balance, heating and dissolving to accurately prepare a CTAB solution of 0.001M;
weighing 0.2g of sulfonated humic acid sample, adding the sulfonated humic acid sample into 500mL of distilled water, swelling for 12 hours, and fixing the volume to 1L;
diluting 10mL of sulfonated humic acid sample solution with 30mL of distilled water, and titrating by using a 0.001M CTAB solution;
measuring the conductivity in the titration by using a conductivity meter until the conductivity is terminated when a volume curve of the CTAB solution is obviously bent;
and calculating the sulfonation degree = 103CV/m × 100%, C is CTAB concentration (mol/L), V is the volume (L) of turning point CTAB, and m is the mass (g) of lignite sulfonated humic acid.
Surface tension measurement
1% (w/v) of humic acid/sulfonated humic acid was prepared accurately and measured using a SITA t-100 surface tension meter.
Suspended matter determination
Adding 1g of dried humic acid/sulfonated humic acid into 50mL of distilled water, stirring for 10 minutes, and standing for 10 minutes;
centrifuging, and drying the precipitate in a drying oven for 1 hour;
weighing the mass of the dried precipitate;
calculated suspension rate =1 g-mass of precipitate after drying (g)/1 g × 100%
Example 2 preparation of potassium humate from lignite
Crushing the lignite into fine particles with the particle size of below 15 meshes by using a crusher;
adding fine particles to 0.6 times the mass of 20% H2O2Stirring the solution for 30 minutes at 50 ℃;
adding the obtained mixture into 1.5 times of KOH aqueous solution with the mass of 1.5%, and continuously stirring for 30 minutes at the temperature of 60 ℃;
centrifuging to remove solids, filtering, and adding concentrated HCI into the obtained filtrate with stirring to adjust pH until a large amount of black precipitate is separated out;
and filtering and drying the separated precipitate to obtain a filter cake, namely the potassium humate of lignite.
Further, upon verification by the applicant, H2O2Oxidation is not an essential step, removal of which reduces the yield by about 10%; in practice, this step may be omitted depending on the composition of the starting materials, or other known oxidation methods, such as nitric acid oxidation, may be used instead as necessary.
Example 3 preparation of sulfonated lignite potassium humate
Dissolving potassium humate of lignite in 10 times of water by mass, and adding 1% of H by mass2SO4And 4% by mass of K2SO3Reacting for 2 hours at 50 ℃;
and drying the solution to obtain a sulfonated lignite potassium humate product (1).
Use 8% H2SO4And (3) sulfonating under similar conditions to obtain a sulfonated potassium montanate product (2).
Using 5% K2SO3And (3) sulfonating under similar conditions to obtain a sulfonated potassium montanate product (3).
Use of 3% H2SO4And 3% of K2SO3And (4) sulfonating under similar conditions to obtain a sulfonated potassium montanate product (4).
Example 4 sulfonated lignite potassium humate Performance test results
Sulfonation degree test results:
surface tension test results
Results of suspension test
In addition, the product (4) is supplemented with 5% of lignosulfonate as a dispersant, and the result shows that the suspension performance of the product reaches only 90.4%, and the introduction of the lignosulfonate not only increases the cost, but also has potential damage to soil or plants.
Using 1% by mass of H2SO4And 4% by mass of K2SO3The sulfonation effect is optimal, although the sulfonation degree, the surface tension and the suspension performance are slightly over 8 percent of sulfuric acid, the alkalization step (or the time/alkali addition amount used in the alkalization step) in the preparation of the fertilizer by using the sulfuric acid sulfonation product is omitted, and the problems of local dehydration and the like in the sulfuric acid sulfonation are avoided. The product has good water solubility/dispersibility, and can effectively prevent the plus or minus hardening of natural peat.
Example 5
The soil conditioner containing humic acid comprises the following components in percentage by weight:
30.0 percent of organic fertilizer
Humic acid 20.0%
CaO 20.0%
MgO 15.0%
The pH value of the soil conditioner is 9.0-12.0;
grinding the sulfonated lignite humic acid product (product 1), adding a calcium-magnesium fertilizer, uniformly mixing and grinding the mixture, and micronizing the mixture until the particle size (the rate of passing through a 60-mesh screen is greater than or equal to 90.0 percent) to obtain the humic acid-containing soil conditioner.
Example 6
The soil conditioner containing humic acid comprises the following components in percentage by weight:
30.0 percent of organic fertilizer
Humic acid 20.0%
CaO 20.0%
MgO 15.0%
The pH value of the soil conditioner is 9.0-12.0;
grinding the sulfonated lignite humic acid product (product 1), adding a calcium-magnesium fertilizer, uniformly mixing and grinding the mixture, and micronizing the mixture until the particle size (the rate of passing through a 60-mesh screen is greater than or equal to 90.0 percent) to obtain the humic acid-containing soil conditioner.
Example 7
Test material and method 1, test soil conditioner
The soil conditioner produced by Zhejiang Fengyu ecological technology Limited company is as shown in examples 5 and 6.
2. Test soil
The soil to which the test point belongs is located in the rock head town rock head village in Pujiang county of Jinhua city in the middle of Zhejiang province, the area belongs to the subtropical monsoon region, and the test point is warm and moist, clear in four seasons, abundant in rainfall and excellent in climate environment. The single-season rice is planted for years, and the production management technical capacity is strong. The test plots are acid obstacle plots, the soil is plus or minus yellow silt, the distribution of the nutrient content of the plots is uniform, and the difference of the fertility level is small. The soil physical and chemical properties at the test points are shown in the following table 1.
TABLE 1 test Point soil types and physicochemical Properties
3. Test site and test crop and variety
The test site is arranged in the rock head town of Pujiang county, Jinhua city, Zhejiang province. The test variety is rice early 390 th.
4. Assay design and method
The test was conducted with three treatments:
and (4) treatment 1, namely comparison treatment, wherein a conventional fertilization mode is adopted. One-time base fertilizer is prepared by applying lOOkg Huidoli formula compound fertilizer (15-6-9, produced by Huidoli agricultural capital Co., Ltd.) to each mu; secondary fertilizer application: and (3) fertilizing urea 25 kg/mu once and fertilizing potassium chloride 2 kg/mu once.
Treatment 2 test treatment, soil conditioner was applied in 2 applications on a regular fertilization basis (example 5). 120kg/667m of soil conditioner is uniformly applied before ploughing2After the rice is harvested, uniformly applying 80kg/667/667m2The total usage is 200 kg/667m2. The time interval between the application and the removal of the soil conditioner and the application of the base fertilizer needs at least more than 1 week.
Treatment 3 test treatment, soil conditioner was applied in 2 applications on a regular fertilization basis (example 6). 120kg/667m of soil conditioner is uniformly applied before ploughing2After the rice is harvested, uniformly applying 80kg/667m2The total usage is 200 kg/667m2. The time interval between the application and the removal of the soil conditioner and the application of the base fertilizer needs at least more than 1 week.
Each treatment of the experiment was repeated 3 times, and the cell area was 35m2And randomly arranging and setting a protection row. Meanwhile, small ridges are built according to requirements, single-row and single-irrigation are carried out, and the small ridges are wrapped by films to prevent leakage, so that the accuracy of test data is ensured, and the yield of the rice in each cell is independently calculated after the rice is harvested.
5. Time of execution of the test
2016-2018, and planting the rice continuously for three years according to the management of a local rice typical planting system. The rice test management status every year is as follows:
sowing in 2016, 4 months and 8 days, namely early seedling cultivation in a middle shed, soil preparation in 27 days in 4 months, ditch opening, ridge forming and water drainage for harrowing, and mulching film treatment on the ridges in 10 days in 5 months to prevent water leakage of each cell. Applying base fertilizer in 11 days in 5 months, manually harrowing, manually transplanting seedlings in 14 days in 5 months, wherein the row spacing and the plant spacing are 30cm x12cm, topdressing is performed for 2 times in the whole growth period, manual weeding is performed for 3 times, and field drying is performed for one time. After harvesting in 8 months and 1 day, no serious natural disasters occur in the whole test process.
Seeding in 2017 in 4 months and 7 days in the mode of raising seedlings in a middle shed early, preparing soil in 25 days in 4 months, opening a canal, ridging, discharging water and harrowing, and treating with mulching films in 9 days in 5 months to re-ridging to prevent water and fertilizer from flowing in each cell. Applying base fertilizer in 5 months and 10 days, manually harrowing, manually transplanting seedlings in 5 months and 13 days, wherein the row spacing and the plant spacing are 30cm x12cm, topdressing is performed for 2 times in the whole growth period, artificial weeding is performed for 3 times, and the field is dried once. After harvesting in 7 months and 30 days, no serious natural disasters occur in the whole test process.
Seeding in 2018, 4-month and 10-day period, namely raising seedlings in a middle shed in a dry mode, preparing soil, opening a canal, ridging and discharging water for raking the soil in 28-day period 4-month period, and treating the soil with mulching films for 11-month period 5 to re-ridging to prevent water and fertilizer from flowing in each cell. Applying base fertilizer in 5-month and 12-day period, manually harrowing, manually transplanting seedlings in 5-month and 14-day period, wherein the row spacing and the plant spacing are 30cmX12cm, the full-growth topdressing is performed for 2 times, the artificial weeding is performed for 3 times, and the field is dried in the sun once. After harvesting in 8 months and 3 days, no serious natural disasters occur in the whole test process.
Second, test results and analysis
1. Influence of soil conditioner on rice yield and yield increase
TABLE 2 influence of soil conditioners on Rice yield traits (2016)
The data in the table show that after the test fertilizer is applied, the yield of the rice is increased, and compared with the conventional fertilizer, the yield increase amplitude of the treatment 3 reaches 20.9%, and the yield increase amplitude of the treatment 2 reaches 38.5%. The significance analysis of the difference among the treatments is carried out by DPS statistical analysis software, and the p value is 0.0087 and less than 0.01, which indicates that the difference reaches a very significant level.
The data of the 2016 year test are analyzed statistically as follows:
table 32016 annual test data statistical analysis table
TABLE 4 influence of soil conditioners on Rice yield traits (2017)
The data in the table show that after the test fertilizer is applied, the yield of the rice is increased, and compared with the conventional fertilizer, the yield increase amplitude of the treatment 3 is 26.8%, and the yield increase amplitude of the treatment 2 is 39.6%.
2. Influence of humic acid-containing soil conditioner on pH value of soil and cation exchange capacity
After harvesting, soil samples of each plot were collected, air-dried, ground, and measured for pH and cation exchange capacity, with the results as given in the table below.
TABLE 5 pH of soil and cation exchange amount
3. Influence of humic acid-containing soil conditioner on soil exchangeable aluminum, available manganese and base saturation
After harvesting, soil samples of each plot were collected, air-dried, ground, and measured for soil exchangeable aluminum, available manganese, and salt base saturation, with the results as given in the table below.
TABLE 6 influence of soil exchangeable aluminum (2018)
The data in the table above show that the soil conditioner can be used to reduce the content of soil exchangeable aluminum. Compared with the control treatment, the content of exchangeable aluminum in the soil of the treatment 3 is reduced by 55.4 percent, and the content of exchangeable aluminum in the soil of the treatment 2 is reduced by 59.4 percent.
TABLE 7 influence of effective manganese in soil (2018)
The data in the table above show that the soil conditioner can reduce the content of available manganese in the soil. Compared with the control treatment, the effective manganese content of the soil of the treatment 3 is reduced by 26.3 percent at most, and the effective manganese content of the soil of the treatment 2 is reduced by 28.4 percent at most.
TABLE 8 influence of soil base saturation (2018)
The data above show that soil base saturation can be improved using soil conditioners. The treatment 3 showed 11.5% increase in saturation of soil bases and the treatment 2 showed 19.8% increase in saturation of soil bases compared to the control treatment.
Third, result and discussion
1. Compared with the contrast treatment without applying the soil conditioner, the application of the soil conditioner can increase the yield of the rice by 20.9-30.2 percent on average, and has better application prospect.
2. Compared with the control treatment without applying the soil conditioner, the application of the soil conditioner can improve the pH value, the cation exchange capacity and the soil base saturation of the acid soil, reduce the content of soil exchangeable aluminum and effective manganese, enhance the soil tiltability and fertilizer retention capacity and be beneficial to the improvement of the acid soil.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention, including any reference to the above-mentioned embodiments. Various modifications to these embodiments will be readily apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. The soil conditioner containing humic acid is characterized by comprising the following active ingredients in percentage by mass:
20.0 to 40.0 percent of organic fertilizer
Humic acid 8.0-25%
CaO 15.0-30.0%
MgO 8.0-20.0%
The pH value of the soil conditioner is 9.0-12.0; the humic acid is sulfonated lignite humic acid which is prepared by sulfonating lignite humic acid;
the preparation method of the sulfonated lignite humic acid comprises the following steps:
1) crushing the lignite into fine particles with the particle size of below 15 meshes by using a crusher;
2) adding fine particles to 0.6 times the mass of 20% H2O2Stirring the solution for 30 minutes at 50 ℃;
3) adding the obtained mixture into 1.5 times of KOH aqueous solution with the mass of 1.5%, and continuously stirring for 30 minutes at the temperature of 60 ℃;
4) centrifuging to remove solids, filtering, and adding concentrated HCI into the obtained filtrate with stirring to adjust pH until a large amount of black precipitate is separated out;
5) filtering and drying the precipitated precipitate to obtain a filter cake, namely lignite humic acid;
6) dissolving lignite humic acid in 10 times of water by mass, and adding 1% by mass of H based on 100% by mass of lignite humic acid2SO4And 4% by mass of K2SO3Reacting for 2 hours at 50 ℃;
7) and drying the solution to obtain the sulfonated lignite humic acid.
2. The humic acid-containing soil conditioner according to claim 1, which comprises the following active ingredients in percentage by mass:
25.0 to 35.0 percent of organic fertilizer
Humic acid 10.0-20%
CaO 15.0-25.0%
MgO 10.0-15.0%
The pH value of the soil conditioner is 9.0-12.0; the humic acid is sulfonated lignite humic acid which is prepared by sulfonating lignite humic acid.
3. The humic acid-containing soil conditioner of claim 1, wherein the organic fertilizer is one or a mixture of fermented chicken manure, fermented straw and wormcast.
4. A process for the preparation of a humic acid containing soil conditioner as claimed in any one of claims 1 to 3 which comprises the steps of:
1) crushing the lignite into fine particles with the particle size of below 15 meshes by using a crusher;
2) adding fine particles to 0.6 times the mass of 20% H2O2Stirring the solution for 30 minutes at 50 ℃;
3) adding the obtained mixture into 1.5 times of KOH aqueous solution with the mass of 1.5%, and continuously stirring for 30 minutes at the temperature of 60 ℃;
4) centrifuging to remove solids, filtering, and adding concentrated HCI into the obtained filtrate with stirring to adjust pH until a large amount of black precipitate is separated out;
5) filtering and drying the precipitated precipitate to obtain a filter cake, namely lignite humic acid;
6) dissolving lignite humic acid in 10 times of water by mass, and adding 1% by mass of H based on 100% by mass of lignite humic acid2SO4And 4% by mass of K2SO3Reacting for 2 hours at 50 ℃;
7) drying the solution to obtain sulfonated lignite humic acid;
8) grinding the sulfonated lignite humic acid prepared in the step 7), adding organic fertilizer, CaO and MgO, uniformly mixing, grinding and micronizing to obtain the soil conditioner.
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Denomination of invention: A soil conditioner containing humic acid and its preparation method Effective date of registration: 20230404 Granted publication date: 20210402 Pledgee: Agricultural Bank of China Limited by Share Ltd. Pujiang County branch Pledgor: Zhejiang Fengyu Ecological Technology Co.,Ltd. Registration number: Y2023980037271 |
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