CN111217651A - Humic acid-containing water-soluble fertilizer suitable for grapes and preparation method and use method thereof - Google Patents
Humic acid-containing water-soluble fertilizer suitable for grapes and preparation method and use method thereof Download PDFInfo
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Abstract
The invention belongs to the field of compound fertilizers. A humic acid-containing water-soluble fertilizer suitable for grapes comprises 50-65% of humic acid and an inorganic compound fertilizer by weight percent; total nitrogen, P2O5、K2The humic acid is a sulfonated lignite humic acid product. The humic acid-containing water-soluble fertilizer suitable for grapes can obviously promote crop growth, improve quality, improve yield and commodity performance, and has obvious effects of increasing yield and value.
Description
Technical Field
The invention belongs to the field of compound fertilizers, and particularly provides a humic acid-containing water-soluble fertilizer suitable for grapes, a preparation method and a use method thereof.
Background
The grape (Vitis vinifera L.) is a woody vine of Vitaceae, and has cylindrical small branch, longitudinal rib, no hair or sparse soft hair, oval leaf, dense or sparse panicle, developed base branch, spherical or elliptical fruit, flowering phase of 4-5 months, and fruit phase of 8-9 months. Although the grapes can be cultivated in various soils (improved), loam and fine sandy loam are the best, and sandy soil has good air permeability but poor fertilizer and water retention capability. Loam is between sandy and clay. The clay soil is poor in air permeability, but good in fertilizer and water retention, slow in nutrient decomposition and absorption, less in spindling phenomenon at the initial stage, less in flower flowing and single-property fruit phenomenon, easy in spindling at the later stage of development, large in cluster fruit grains, but not good in sugar degree and meat quality, and the soil needs to be maintained and improved.
Grapes are similar to most crops in that they require about 17 nutrients for growth: carbon, hydrogen, oxygen, nitrogen, phosphorus, potassium, calcium, magnesium, sulfur, iron, manganese, zinc, copper, boron, molybdenum, chlorine and cobalt, wherein carbon and oxygen in the base are carbon dioxide obtained from air during photosynthesis, hydrogen comes from moisture in soil, and other elements except nitrogen are mostly absorbed from the soil by roots, and the proportion relation is as follows: 94% -99.5% of the fresh crop tissue is made up of air and water combined with carbon, hydrogen and oxygen, and only about 0.5% -6% is the nutrient elements from the soil. The chemical fertilizer mainly provides three elements of nitrogen, phosphorus and potassium, and some fertilizers also contain a large amount of calcium, magnesium and sulfur, and although the effect of the fertilizer is obvious, the fertilizer is easy to cause fertilizer damage when being used excessively. The organic fertilizer has low content of nutrient elements, can be used in large amount, and has improvement effect on physical, chemical and biological properties of soil. In addition, soil conditioners can be added according to the soil conditions, 3 modes of base fertilizer, top dressing and foliar fertilization are mostly adopted for nutrition supplement, and the base fertilizer is used after hibernation or harvesting.
Humic acid is a complex network of macromolecules containing a large number of different functional groups as well as 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. In order to improve the soil of grape planting areas, a more economical and efficient preparation method of potassium humate from lignite is needed.
Disclosure of Invention
In view of the above problems, the inventors have invented a humic acid water-soluble fertilizer suitable for grape planting, which uses a sulfonated lignite humic acid product as a main component, and the sulfonated lignite humic acid product is sulfonated by using hydrogen peroxide and then a small amount of sulfuric acid in combination with sulfite, so that a sulfonated lignite potassium humate with high water solubility/dispersibility can be prepared without using a dispersant. The sulfonated potassium lignite humate is used for grape planting, and a good effect is achieved.
On one hand, the application provides a humic acid water-soluble fertilizer suitable for grape planting, which comprises 50-65% of humic acid and an inorganic compound fertilizer by weight percent; the inorganic compound fertilizer comprises the following components:
the total nitrogen and P2O5、K2The humic acid is a sulfonated lignite humic acid product.
Further, 55-60% of humic acid by weight percentage; the inorganic compound fertilizer comprises the following components:
the total nitrogen and P2O5、K2The humic acid is a sulfonated lignite humic acid product.
Further, the application also provides a preparation method of the sulfonated lignite humic acid product, which 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.
Further, step (2) of adding the fine particles to 0.6 times by mass of 20% H2O2The solution was stirred at 50 ℃ for 30 minutes.
Further, in step (3), the resultant mixture was added to 1.5 times by mass of a 1.5% aqueous solution of KOH, and 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。
In another aspect, the present application provides a method of preparing a water-soluble fertilizer, the method 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 sulfonated lignite humic acid product prepared in the step (7), adding an inorganic compound fertilizer, mixing and stirring to obtain the water-soluble fertilizer.
Further, the application method of the water-soluble fertilizer comprises the steps of applying the humic acid-containing water-soluble fertilizer on the basis of conventional fertilization, and applying the fertilizer in a fruit setting period and a fruit swelling period for 2 times in total, wherein the application amount is 20kg/667 square meter each time, and the application concentration is 150 times of liquid.
The lignite can be produced in various production places, and the indexes of humic acid, water and carbon content of the lignite can be different as long as the lignite conforms to the general definition of the lignite in the industry.
Agents of the invention, e.g. sulfonating agent H2SO4、K2SO3Qualified products of various purities can be selected according to conditions, and are not limited to individual brands or standards.
The fertilizer in the invention comprises fertilizers of various application modes, wherein the fertilizer can contain known fertilizer components which do not conflict with the sulfonated lignite humic acid, including but not limited to trace elements, other organic fertilizers and the like.
Compared with the conventional local fertilization, the application of the humic acid-containing water-soluble fertilizer can increase the yield of the grapes by more than 18.5 percent; can obviously promote the growth of crops, improve the quality, improve the yield and the commodity, and has the obvious effects of increasing the production and the value.
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 of 103CV/m multiplied by 100 percent, C is CTAB concentration (mol/L), V is the volume (L) of turning point CTAB, and m is the mass (g) of the 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;
the suspension percentage was calculated to be 1 g-mass of precipitate after drying (g)/1g × 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:
| product(s) | Product (1) | Product (2) | Product (3) | Product (4) |
| Degree of sulfonation (%) | 18.88 | 18.59 | 6.91 | 10.22 |
Surface tension test results
| Product(s) | Product (1) | Product (2) | Product (3) | Product (4) |
| Surface tension mN/m | 50.74 | 52.36 | 65.56 | 70.21 |
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 is suitable for preparing water-soluble fertilizers.
Example 5
The water-soluble fertilizer comprises humic acid and an inorganic compound fertilizer, and the humic acid product of the sulfonated lignite is 55 percent by weight; the inorganic compound fertilizer comprises the following components:
the total nitrogen and P2O5、K2The humic acid is a sulfonated lignite humic acid product.
Grinding the sulfonated lignite humic acid product (1), adding an inorganic compound fertilizer according to the formula, and mixing and stirring to obtain the water-soluble fertilizer.
Example 6
The water-soluble fertilizer comprises humic acid and an inorganic compound fertilizer, and the humic acid product of the sulfonated lignite is 55 percent by weight; the inorganic compound fertilizer comprises the following components:
the total nitrogen and P2O5、K2The humic acid is a sulfonated lignite humic acid product.
And (3) grinding the sulfonated lignite humic acid product, adding an inorganic compound fertilizer according to the formula, and mixing and stirring to obtain the water-soluble fertilizer.
Example 6 practical Effect of Using humic acid containing sulfonated lignite for grape cultivation
Test materials and designs
1.1 test site and test crop, variety.
The test sites were set at the subsidiary agricultural products of Pujiang Tanfeng, Limited, under xi, Pujiang county, Jinhua, Zhejiang, Lishui, Jinyun, Shuiyun, Shuaishui, Jieyu, county, Dongli, Jieshai grape professional cooperative. The grape variety is: a huge peak.
1.2 basic conditions of the test
The test points are in the middle and east regions of Zhejiang province and are influenced by subtropical humid monsoon climate, the annual temperature is moderate, the rainfall is abundant, the climate environment is superior, the grape industry develops for many years, and the production technology capability is strong. The difference between the soil to be tested and the soil in two places is not large, and the soil type and the physical and chemical properties of each test point are shown in the following table 1:
TABLE 1 two test points soil types and physicochemical Properties
1.3 design of test treatment
The test was conducted with two treatments, respectively:
and (3) conventional fertilization: 100kg/667 square meter of ternary compound fertilizer applied per mu, 15-15-15 nutrient content, produced by Shenzhen Shanba ecological engineering shares, Ltd. The fertilizer consumption accounts for 30% of the base fertilizer, and the additional fertilizer accounts for 70% of the fertilizer in the fruit setting period and the fruit expanding period. And (3) pouring clean water which is equal to the amount of the clean water treated 1 at the same time during top dressing.
Treatment 1: applying a humic acid-containing water-soluble fertilizer (example 6) on the basis of conventional fertilization, and applying the fertilizer in a fruit setting period and a fruit swelling period for 2 times in total, wherein the application amount is 20kg/667 square meter per time, and the application concentration is 150 times of liquid.
And (3) treatment 2: applying a humic acid-containing water-soluble fertilizer (example 5) on the basis of conventional fertilization, and applying the fertilizer in a fruit setting period and a fruit swelling period for 2 times in total, wherein the application amount is 20kg/667 square meter per time, and the application concentration is 150 times of liquid.
Each treatment of the test is repeated for 3 times, the area of each cell is 40 square meters (20 plants), the square meters are randomly arranged, and protection rows are arranged.
1.4 test application time:
pujiang county xi sanders: the first watering is carried out in 19 th in 5 th and 7 th in 2017, the second watering is carried out in 7 th and 7 th in 7 th, picking is started in 27 th in 7 th, harvesting is finished in 16 th in 9 th, and no serious natural disaster occurs in the whole test process.
Jinyunjie comma grape professional cooperative: the first watering is carried out in 5 and 15 months in 2017, the second watering is carried out in 5 and 7 months in 2017, picking is started in 25 and 7 months, harvesting is finished in 15 and 9 months, and no serious natural disaster occurs in the whole test process.
Second, test results and analysis
2.1 statistics of yield
The effect of applying humic acid-containing water-soluble fertilizer (hereinafter referred to as test fertilizer) on the yield traits of grapes is detailed in the following table:
the data in the table show that after the test fertilizer is applied, the yield of the grapes is increased, and compared with the conventional fertilizer application, the large field point of Pujiang county in the mode of treatment 1 for increasing the yield is 22.5%, and the large field point of red silk cloud point is 18.5%; the mode of treatment 2 is better than the mode of treatment 1, and the effect is obvious.
Adopting DPS statistical analysis software to carry out significance analysis, and obtaining a result that the P value of the Pujiang county point is 0.0445 and less than 0.05, which indicates that the significance level is reached; red silk cloud point P value 0.0453, less than 0.05, indicates a significant level was reached.
The statistical analysis of the Pujiang points is as follows:
red silk cloud point statistical analysis is as follows:
2.2 growth potential conditions
The field test shows that the cast-in-place test fertilizer can lead the grapes to grow rapidly, the leaves are dark green, the leaves are large and thick, the diseases are obviously reduced, the peel color is bright, the fruits are large and uniform, the bunch shape is good, and the commodity performance is excellent.
2.3 Effect on grape quality index
And (3) applying a humic acid water-soluble fertilizer. Has certain effect on improving the quality index of the grapes. As can be seen from the table, compared with the conventional fertilization treatment, the treatment 1 increases soluble solids, soluble sugar, Vc, etc. at pu river point by 13.9%, 17.2% and 8.8%, respectively, and decreases total acid by 10.8%, increases soluble solids, soluble sugar, Vc, etc. at yun point by 8.8%, 10.5% and 18.1%, respectively, and decreases total acid by 61.8%; the mode of treatment 2 is better than the mode of treatment 1, and the effect is obvious. The humic acid fertilizer is applied to grapes, the glucose-acid ratio is improved, the taste and flavor are better, and the commodity value is improved.
TABLE 2 influence of humic acid water-soluble fertilizer on grape quality
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 (10)
1. The humic acid-containing water-soluble fertilizer suitable for grapes is characterized by comprising 50-65% of humic acid and inorganic compound fertilizer by weight percent; the inorganic compound fertilizer comprises the following components:
total nitrogen 10-20%
P2O55.0-10.0%
K2O 8.0-15.0%
0.50 to 1.0 percent of zinc
0.50 to 1.0 percent of iron
0.50 to 1.0 percent of magnesium
0.10 to 0.50 percent of boron
0.05 to 0.10 percent of copper
0.05 to 0.10 percent of molybdenum
0.05 to 0.10 percent of manganese;
the total nitrogen and P2O5、K2The humic acid is a sulfonated lignite humic acid product.
2. The humic acid-containing water-soluble fertilizer suitable for grapes according to claim 1, wherein the humic acid is 55-60% by weight; the inorganic compound fertilizer comprises the following components:
total nitrogen is 12-15%
P2O58.0-10%
K2O10 -15%
0.50 to 1.0 percent of zinc
0.50 to 1.0 percent of iron
0.50 to 1.0 percent of magnesium
0.10 to 0.50 percent of boron
0.05 to 0.10 percent of copper
0.05 to 0.10 percent of molybdenum
0.05 to 0.10 percent of manganese;
the total nitrogen and P2O5、K2The humic acid is a sulfonated lignite humic acid product.
3. The humic acid-containing water-soluble fertilizer suitable for grapes according to claim 1 or 2, characterized in that 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.
4. The humic acid-containing water-soluble fertilizer for grapes according to claim 3, wherein the fine particles added in the step (2) are 0.6 times by mass of 20% H2O2The solution was stirred at 50 ℃ for 30 minutes.
5. The humic acid-containing water-soluble fertilizer applicable to grapes according to claim 3 or 4, wherein the mixture obtained in step (3) is added to 1.5 times by mass of a 1.5% KOH aqueous solution, and stirring is continued at 60 ℃ for 30 minutes.
6. A humic acid-containing water-soluble fertilizer suitable for grapes according to any one of claims 3 to 5, wherein in the step (6), lignite humic acid is dissolved in 10 times the mass of water and reacted at 50 ℃ for 2 hours.
7. The humic acid-containing water-soluble fertilizer suitable for grapes according to claim 6, wherein 0.5% by mass of H is used in step (6)2SO4And/or 4% by mass of K2SO3。
8. The humic acid-containing water-soluble fertilizer suitable for grapes according to claim 7, wherein 0.5% by mass of H is used in step (6)2SO4And 4% by mass of K2SO3。
9. A method of producing a water-soluble fertilizer as claimed in any one of claims 1 to 8, the method 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 sulfonated lignite humic acid product prepared in the step (7), adding an inorganic compound fertilizer, mixing and stirring to obtain the water-soluble fertilizer.
10. The use method of the water-soluble fertilizer according to any one of claims 1 to 8, which comprises the steps of applying the water-soluble fertilizer containing humic acid on the basis of conventional fertilization, and pouring the fertilizer in a fruit setting period and a fruit swelling period for 2 times in total, wherein the application amount is 20kg/667 square meter per time, and the pouring concentration is 150 times of liquid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111233550A (en) * | 2020-01-19 | 2020-06-05 | 浙江丰瑜生态科技股份有限公司 | Humic acid water-soluble fertilizer suitable for hickory planting and preparation method and application thereof |
| CN114437367A (en) * | 2022-02-25 | 2022-05-06 | 云南旭光节能有限公司 | Method for producing potassium humate by utilizing lignite humic acid |
| CN116082095A (en) * | 2023-02-24 | 2023-05-09 | 新疆锦华农药有限公司 | Long-acting stable humic acid water-soluble fertilizer and preparation method thereof |
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| CN111233550A (en) * | 2020-01-19 | 2020-06-05 | 浙江丰瑜生态科技股份有限公司 | Humic acid water-soluble fertilizer suitable for hickory planting and preparation method and application thereof |
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| CN114437367A (en) * | 2022-02-25 | 2022-05-06 | 云南旭光节能有限公司 | Method for producing potassium humate by utilizing lignite humic acid |
| CN116082095A (en) * | 2023-02-24 | 2023-05-09 | 新疆锦华农药有限公司 | Long-acting stable humic acid water-soluble fertilizer and preparation method thereof |
| CN116082095B (en) * | 2023-02-24 | 2024-02-02 | 新疆锦华农药有限公司 | Long-acting stable humic acid water-soluble fertilizer and preparation method thereof |
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