CN111116260A - Water-soluble fertilizer containing humic acid and preparation method thereof - Google Patents
Water-soluble fertilizer containing humic acid and preparation method thereof Download PDFInfo
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- CN111116260A CN111116260A CN202010003643.7A CN202010003643A CN111116260A CN 111116260 A CN111116260 A CN 111116260A CN 202010003643 A CN202010003643 A CN 202010003643A CN 111116260 A CN111116260 A CN 111116260A
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- humic acid
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- lignite
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- soluble fertilizer
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G22/00—Cultivation of specific crops or plants not otherwise provided for
- A01G22/05—Fruit crops, e.g. strawberries, tomatoes or cucumbers
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
- C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
Abstract
The invention belongs to the field of fertilizers. The invention provides a humic acid-containing water-soluble fertilizer which comprises sulfonated lignite humic acid, a wetting agent and a disintegrating agent, wherein the sulfonated lignite humic acid is prepared by using sulfuric acid and potassium sulfite sulfonated humic acid.
Description
Technical Field
The invention belongs to the field of fertilizers, and particularly provides a method for preparing sulfonated lignite humic acid, a sulfonated lignite humic acid product prepared by the method and a corresponding water-soluble fertilizer.
Background
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 addition, auxiliaries such as a disintegrating agent, a dispersing agent, a wetting agent and the like which are required to be added into the water-soluble fertilizer containing humic acid also need to be optimized correspondingly
Therefore, the method has the needs of further improving the humic acid preparation and humic acid sulfonation processes of coal, optimizing the formula of the auxiliary agent and preparing corresponding cheap and efficient water-soluble fertilizer.
Disclosure of Invention
In order to solve the problems, the inventor tries various sulfonation modes of lignite humic acid, and finds that the sulfonation effect and the dispersion effect can be effectively improved by using a small amount of sulfuric acid to be matched with sulfite for sulfonation, and even sulfonated lignite humic acid with high water solubility/dispersibility can be prepared without using an oxidation step and a dispersing agent. When the humic acid is used for preparing the fertilizer, the use is convenient and the fertilizer efficiency is good.
In one aspect, the present application provides a water-soluble fertilizer containing sulfonated lignite humic acid, comprising sulfonated lignite humic acid, a wetting agent and a disintegrant.
Further, the wetting agent is SDS, and the disintegrating agent is sodium carbonate.
Furthermore, the adding amount of SDS is 5% of the mass of the humic acid of the sulfonated lignite, and the adding amount of sodium carbonate is 3% of the mass of the humic acid of the sulfonated lignite.
Further, the sulfonated lignite humic acid is prepared by the following method:
(1) crushing lignite into fine particles by using a crusher; (2) adding the fine particles into NaOH aqueous solution, and stirring; (3) 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; (4) filtering the separated precipitateDrying to obtain lignite humic acid; (5) dissolving humic acid of lignite in water, adding H2SO4And/or K2SO3Reacting; (6) and drying the solution to obtain a sulfonated lignite humic acid product.
Further, the aqueous solution of NaOH in step (2) was 2 times the mass of the aqueous solution of 2% NaOH, and stirring was continued at 60 degrees celsius for 20 minutes.
Further, in the step (5), 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, 1% by mass of H was used in the step (5)2SO4And/or 4% by mass of K2SO3。
Further, 1% by mass of H was used in the step (5)2SO4And 4% by mass of K2SO3。
In another aspect, the application provides an application of the fertilizer in pepper planting.
In another aspect, the present application provides a method for preparing sulfonated lignite humic acid, comprising:
(1) crushing lignite into fine particles by using a crusher; (2) adding the fine particles into 2 times of NaOH aqueous solution with the mass of 2%, and stirring; (3) 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; (4) filtering and drying the precipitated precipitate to obtain lignite humic acid; (5) dissolving humic acid 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 ℃; (6) and drying the solution to obtain a sulfonated lignite humic acid product.
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、K2SO3Sodium carbonate and urea as disintegrating agent, Tween, span, SDS and other wetting agent may be selected according to different purity and are not limitedIn a separate brand or standard.
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, and the fertilizer comprises but is not limited to trace elements, nitrogen, phosphorus, potassium, other organic fertilizers and the like.
Examples
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 dried precipitate;
the suspension percentage was calculated to be 1 g-mass of precipitate after drying (g)/1g × 100%
Example 2 preparation of humic acid from lignite
Crushing the lignite into fine particles with the particle size of below 15 meshes by using a crusher;
adding the fine particles into 2 times of NaOH aqueous solution with the mass of 2%, and continuously stirring for 20 minutes at 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 precipitated precipitate to obtain a filter cake, namely the lignite humic acid.
Example 3 preparation of humic acid of sulfonated lignite
Dissolving lignite humic acid 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 humic acid product (1).
Use 8% H2SO4And (3) sulfonating under similar conditions to obtain a sulfonated lignite humic acid product (2).
Using 5% K2SO3And (3) sulfonating under similar conditions to obtain a sulfonated lignite humic acid product (3).
Use of 3% H2SO4And 3% of K2SO3And (4) sulfonating under similar conditions to obtain a sulfonated lignite humic acid product (4).
Example 4 humic acid Performance test results for sulfonated lignite
Sulfonation degree test results:
| product(s) | Product (1) | Product (2) | Product (3) | Product (4) |
| Degree of sulfonation (%) | 18.05 | 18.21 | 7.57 | 9.33 |
Surface tension test results
Results of suspension test
In addition, the product (3) is supplemented with PEG 60005% or lignosulfonate 4% as a dispersing agent, and the result shows that the suspension performance only reaches 89.2% and 92.5%, while the introduction of PEG6000 and 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 best, although the sulfonation degree is slightly lower than 8 percent of sulfuric acid, the surface tension and the suspension performance exceed 8 percent of sulfuric acid, and the sulfuric acid sulfonation is omittedThe alkalization step (or the time/alkali addition amount used in the alkalization step) in the preparation of the fertilizer by the product is reduced, and the problems of local dehydration and the like in sulfuric acid sulfonation are avoided. The product has good water solubility/dispersibility and is suitable for preparing water-soluble fertilizers.
SDS (sodium dodecyl sulfate) accounting for 5 percent of the mass of the sulfonated lignite humic acid and sodium carbonate accounting for 3 percent of the mass of the sulfonated lignite humic acid are added into various sulfonated lignite humic acid products to prepare water-soluble fertilizer products.
Example 5 practical Effect of sulfonated lignite humic acid for Pepper planting
The partial research is carried out by the institute of environmental resources and soil fertilizers of agricultural science institute of Zhejiang province, except for product number, the following data provide 1.1 test site and test crops and varieties
The test sites were set in the Tuwobao demonstration base of Bingshangchun Temple and the Jinjiang Jinhua city, Pujiang county, Zhejiang province and the Shaoxing city, Chingjinbo family farm. The pepper variety is as follows: zhe jiao No. 3.
1.2 basic conditions of the test
The test points are located 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 vegetable 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 as follows:
1.3 design of test treatment
The test was conducted with two treatments, respectively:
treatment 1: applying water soluble fertilizer containing sulfonated lignite humic acid product (4) on the basis of conventional fertilizer application (50 Kg of Barda compound fertilizer (15-15-15) produced by Shenzhen Barda ecological engineering Co., Ltd.) per mu, applying 3 times of water application in seedling stage, initial stage of fruiting and full period of fruiting after field planting and survival, wherein the total dosage is 30Kg/667m2And pouring liquid with the concentration of 160 times. .
And (3) treatment 2: conventional fertilization (50 Kg of compound fertilizer for Barbada field is applied per mu (15-15-15) water soluble fertilizer containing sulfonated lignite humic acid product (1) is applied on the basis of Shenzhen Shanggan ecological engineering Co., Ltd), the water soluble fertilizer is applied in the seedling stage, the initial stage of fruiting and the full stage of fruiting after the planting survival for 3 times, and the total dosage is 30Kg/667m2And pouring liquid with the concentration of 160 times.
Each treatment of the test is repeated for 3 times, the area of a cell is 35 square meters, the cells are randomly arranged, and protection rows are arranged.
1.4 test application time:
pujiang county item hometown head: transplanting in 2017 in 5-month and 22-day period, picking in 6-month and 20-day period, harvesting in 9-month and 18-day period, and no serious natural disaster occurs in the whole test process.
Jinbo family farm: transplanting in 2017 in 23 months, picking in 22 days in 6 months, harvesting in 10 days in 9 months, and no serious natural disasters occur in the test process.
2.1 statistics of yield
Adopting DPS statistical analysis software to carry out significance analysis, and indicating that the P value of Pujiang county point is 0.0227 and less than 0.05, which indicates that the significance level is reached; the Shaoxing-panjiang point P value is 0.0293 and less than 0.05, which indicates that the significant level is achieved. The yield of product (1) at the same amount is significantly higher than that of product (4).
The statistical analysis of the Pujiang points is as follows:
the shaoxing point statistical analysis is as follows:
Claims (10)
1. a water-soluble fertilizer containing humic acid is characterized by comprising sulfonated lignite humic acid, a wetting agent and a disintegrating agent.
2. The water-soluble fertilizer according to claim 1, wherein said wetting agent is SDS and said disintegrating agent is sodium carbonate.
3. The water-soluble fertilizer according to claim 2, wherein the amount of SDS added is 5% by mass of humic acid of sulfonated lignite, and the amount of sodium carbonate added is 3% by mass of humic acid of sulfonated lignite.
4. A water-soluble fertilizer according to any one of claims 1 to 3, characterized in that the sulphonated lignite humic acid is prepared by the following process:
(1) crushing lignite into fine particles by using a crusher; (2) adding the fine particles into NaOH aqueous solution, and stirring; (3) 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; (4) filtering and drying the precipitated precipitate to obtain lignite humic acid; (5) dissolving humic acid of lignite in water, adding H2SO4And/or K2SO3Reacting; (6) and drying the solution to obtain a sulfonated lignite humic acid product.
5. The water-soluble fertilizer according to claim 4, characterized in that the aqueous NaOH solution in the step (2) is 2 times the mass of the 2% aqueous NaOH solution, and stirring is continued at 60 ℃ for 20 minutes.
6. The water-soluble fertilizer according to claim 5, characterized in that in the step (5), the lignite humic acid is dissolved in 10 times the mass of water and reacted at 50 ℃ for 2 hours.
7. Water-soluble fertilizer according to claim 6, characterized in that 1% by mass of H is used in step (5)2SO4And/or 4% by mass of K2SO3。
8. Water-soluble fertilizer according to claim 7, characterized in that 1% by mass of H is used in step (5)2SO4And 4% by mass of K2SO3。
9. Use of a water-soluble fertilizer according to any one of claims 1-8 in pepper planting.
10. A method for preparing sulfonated lignite humic acid is characterized by comprising the following steps:
(1) crushing lignite into fine particles by using a crusher; (2) adding the fine particles into 2 times of NaOH aqueous solution with the mass of 2%, and stirring; (3) 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; (4) filtering and drying the precipitated precipitate to obtain lignite humic acid; (5) dissolving humic acid 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 ℃; (6) and drying the solution to obtain a sulfonated lignite humic acid product.
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Cited By (2)
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| CN111217651A (en) * | 2020-02-13 | 2020-06-02 | 浙江丰瑜生态科技股份有限公司 | Humic acid-containing water-soluble fertilizer suitable for grapes and preparation method and use method thereof |
| 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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| 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 |
| CN111233550B (en) * | 2020-01-19 | 2021-11-23 | 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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