CN115246751A - Preparation method of high-hard water resistance organic water-soluble bacterial fertilizer - Google Patents
Preparation method of high-hard water resistance organic water-soluble bacterial fertilizer Download PDFInfo
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- CN115246751A CN115246751A CN202110455668.5A CN202110455668A CN115246751A CN 115246751 A CN115246751 A CN 115246751A CN 202110455668 A CN202110455668 A CN 202110455668A CN 115246751 A CN115246751 A CN 115246751A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
- C05C5/04—Fertilisers containing other nitrates containing calcium nitrate
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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
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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
- C05G3/80—Soil conditioners
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Soil Sciences (AREA)
- Fertilizers (AREA)
Abstract
A preparation method of a high hard water resistance organic water-soluble bacterial fertilizer comprises the steps of carrying out two-stage centrifugal separation on humic acid extract, carrying out graft copolymerization reaction under the conditions of certain temperature, pressure and initiator, carrying out sulfonation and complex reaction under the conditions of certain temperature and pressure, and controlling the temperature of a fluidized bed compound and the water content of a product according to different microbial inoculum temperature tolerance conditions to prepare the high hard water resistance organic water-soluble bacterial fertilizer. According to the invention, humic acid is subjected to sulfonation reaction, so that the water solubility and the anticoagulation of the product are improved, and the hard water resistance of the product is improved; the humic acid salt is used as a carrier to carry out composite reaction with the bacterial manure and the microbial agent on the fluidized bed, so that the humic acid water-soluble fertilizer is compounded with the trace elements, multiple effects of one fertilizer are realized, the application is convenient, the soil remediation and the prevention of root diseases can be realized, the complete supply of the large and medium trace elements can be realized, the crop yield is improved, and the quality of crops is improved.
Description
Technical Field
The invention relates to the field of novel fertilizer production and research and development, and particularly relates to a preparation method of a high-hard water resistance organic water-soluble bacterial fertilizer.
Background
China is the largest country of use and production of chemical fertilizers in the world, but continuous excessive use of chemical fertilizers causes the problems of large-area soil hardening, soil fertility reduction, crop yield reduction, quality reduction, soil microorganism unbalance, increasingly serious soil-borne diseases and the like in farmlands in China. Because the irrigation water quality in China is high in salt content, soluble organic matters, particularly humates, quickly flocculate to cause irrigation pipelines to be blocked, organic water-soluble fertilizers which can effectively improve the quality of crops cannot be applied, and the organic water-soluble fertilizers are not suitable for being applied in water and fertilizer integrated facilities and are not stable enough in effect.
Disclosure of Invention
According to the background, the bacterial manure microbial agent is added to the fulvic acid carrier to improve the soil granular structure and promote the bacterial manure microorganisms to colonize and propagate in soil, so that the mutual promotion of the bacterial manure microorganisms and the soil microbial agent is achieved, the fertilizer efficiency is more stable and durable, and the application is easier, and the purpose of water-fertilizer integrated facility fertilization is met.
A preparation method of a high hard water resistance organic water soluble bacterial fertilizer comprises the following steps:
s1: extracting weathered coal and alkali (sodium hydroxide or potassium hydroxide) slurry in a reaction kettle at the temperature of 80-100 ℃ to obtain humic acid extracting solution;
s2: performing secondary centrifugal separation on the humic acid extract to ensure that the content of solid matters (water-insoluble substances) in the humic acid salt solution is less than 1.5 percent;
s3: the humate solution obtained in the step S2 is subjected to triple effect concentration to increase the concentration of the humate solution to 18-22%, and then reacts with acrylic acid and sodium sulfite in a reaction kettle at the temperature of 80-100 ℃ and under the condition of normal pressure and an initiator for 3 hours, so that the acrylic acid and the sodium sulfite react with carboxyl groups, phenolic hydroxyl groups and other groups in the humic acid, and the mass fraction ratio of the materials is as follows: humic acid: acrylic acid: sodium sulfite =100, solid content of humate: the initiator is 100;
s4: and (3) reacting the product obtained in the step (S3) with sodium pyrosulfite in a reaction kettle at the temperature of 60-80 ℃ and under normal pressure for 2 hours, wherein the mass fraction ratio of the product of the step (S2) to the sodium pyrosulfite is as follows: 100, and (c) a water-soluble polymer compound;
s5: and (3) reacting the product in the step (S4) with copper sulfate, ferrous sulfate, zinc sulfate, magnesium chloride and calcium nitrate in a reaction kettle for 2 hours at the temperature of 80-100 ℃ and under the normal pressure condition, wherein the mass percentage of the product in the step (S4) is 100: copper sulfate 2 to 5: ferrous sulfate 2 to 5: 2-5 of zinc sulfate: 2 to 5 portions of magnesium chloride;
s6: and (3) spray-drying the humate solution obtained in the step (S5) to obtain humate powder, carrying out compound reaction on the humate powder and a microbial agent (such as bacillus subtilis robustum, bacillus amyloliquefaciens, bacillus mucilaginosus robustum and the like) by using a fluidized bed, and controlling the compound temperature of the fluidized bed to be 55-75 ℃ according to different microbial agent temperature tolerance conditions to obtain a qualified product.
Further, the initiator in S1 is 4% of potassium persulfate;
further, the secondary centrifugal separation equipment used in step 2 is a horizontal centrifuge or a butterfly centrifuge;
further, the water content of the product in the S6 is 5-12%.
The humate of the invention can improve water solubility and anticoagulation property through sulfonation reaction, and improve the hard water resistance of the product, and the humate adopts weathered coal, belongs to natural organic active substances, and can reduce pollution, improve soil, improve fertilizer efficiency and improve crop quality.
Detailed Description
In order to clearly understand the technical scheme of the invention, the following detailed description of the specific embodiments of the invention is provided in connection with the examples. The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
A preparation method of a high hard water resistance organic water soluble bacterial fertilizer comprises the following steps:
s1: extracting weathered coal and alkali (sodium hydroxide or potassium hydroxide) slurry in a reaction kettle at the temperature of 80 to 100 ℃ to obtain humic acid extract;
s2: performing secondary centrifugal separation on the humic acid extract to ensure that the content of solid matters (water-insoluble substances) in the humic acid salt solution is less than 1.5 percent;
s3: the humate solution obtained in the step S2 is subjected to triple effect concentration to increase the concentration of the humate solution to 18-22%, and then reacts with acrylic acid and sodium sulfite in a reaction kettle at the temperature of 80-100 ℃ and under the condition of normal pressure and an initiator for 3 hours, so that the acrylic acid and the sodium sulfite react with carboxyl groups, phenolic hydroxyl groups and other groups in the humic acid, and the mass fraction ratio of the materials is as follows: humic acid: acrylic acid: sodium sulfite =100, solid content of humate: the initiator is 100;
s4: and (3) reacting the product obtained in the step (S3) with sodium pyrosulfite in a reaction kettle at the temperature of 60-80 ℃ and under normal pressure for 2 hours, wherein the mass fraction ratio of the product of the step (S2) to the sodium pyrosulfite is as follows: 100, and (c) a water-soluble polymer compound;
s5: and (3) reacting the product in the step (S4) with copper sulfate, ferrous sulfate, zinc sulfate, magnesium chloride and calcium nitrate in a reaction kettle for 2 hours at the temperature of 80-100 ℃ and under the normal pressure condition, wherein the mass percentage of the product in the step (S4) is 100:2 to 5 parts of copper sulfate: ferrous sulfate 2 to 5: 2-5 of zinc sulfate: 2 to 5 portions of magnesium chloride;
s6: and (3) spray-drying the humate solution obtained in the step (S5) to obtain humate powder, carrying out compound reaction on the humate powder and microbial agents (such as bacillus subtilis bud, bacillus amyloliquefaciens, bacillus mucilaginosus-like bud and the like) by using a fluidized bed, and controlling the compound temperature of the fluidized bed to be 55-75 ℃ according to different microbial agent temperature tolerance conditions to obtain qualified products.
Preferably, the initiator in S1 is 4% of potassium persulfate;
preferably, the secondary centrifugal separation equipment used in step 2 is a horizontal centrifuge or a butterfly centrifuge;
preferably, the water content of the product in the S6 is 5-12%.
Compared with the market products, the product of the invention:
| product name | Free humic acid | Water insoluble substance | pH value | Dissolution rate | Hard water resistance |
| Products of the invention | >65% | <1.5% | 7.0-7.5 | 30s | Hard water resistance and flocculation resistance |
| Market competitive products | >60% | <5.0% | >10 | >2min | Hard water and flocculation resistance |
| Common products in the market | >50% | <15.0% | >10 | >2min | Hard water and flocculation resistance |
According to the invention, the humate is subjected to sulfonation reaction, so that the water solubility and the anticoagulation can be improved, the hard water resistance of the product is improved, the humate is used as a carrier to perform composite reaction with bacterial manure and a microbial agent on a fluidized bed, trace elements are added in the humic acid water-soluble fertilizer in a composite manner, one fertilizer with multiple effects is realized, the application is convenient, meanwhile, the soil remediation can be considered, the root diseases can be prevented, the complete supply of large and medium trace elements can be realized, and the quality of crops can be improved while the yield of the crops is improved.
The foregoing is a preferred embodiment of the present invention, and all equivalent changes or modifications in the structure, characteristics and principles of the invention described in the claims of the present application are included in the scope of the present application.
Claims (4)
1. A preparation method of a high hard water resistance organic water soluble bacterial fertilizer is characterized by comprising the following steps:
s1: extracting weathered coal and alkali (sodium hydroxide or potassium hydroxide) slurry in a reaction kettle at the temperature of 80 to 100 ℃ to obtain humic acid extract;
s2: performing secondary centrifugal separation on the humic acid extract to ensure that the content of solid matters (water-insoluble substances) in the humic acid salt solution is less than 1.5 percent;
s3: and (3) increasing the concentration of the humate solution obtained in the S2 to 18-22% through triple effect concentration, and then reacting the humate solution with acrylic acid and sodium sulfite in a reaction kettle for 3 hours at the temperature of 80-100 ℃ under the normal pressure and under the condition of an initiator, wherein the mass fraction ratio of the materials is as follows: humic acid: acrylic acid: sodium sulfite =100, 0.5: the initiator is 100;
s4: and (2) reacting the product obtained in the step (S3) with sodium pyrosulfite in a reaction kettle at the temperature of 60-80 ℃ and under normal pressure for 2 hours, wherein the mass fraction ratio of the product obtained in the step (S2) to the sodium pyrosulfite is as follows: 100, and (c) a step of;
s5: and (3) reacting the product in the step S4 with copper sulfate, ferrous sulfate, zinc sulfate, magnesium chloride and calcium nitrate in a reaction kettle for 2 hours at the temperature of 80-100 ℃ and under normal pressure, wherein the mass fraction of the product in the step S4 is 100:2 to 5 parts of copper sulfate: 2 to 5 of ferrous sulfate: 2-5 of zinc sulfate: 2 to 5 parts of magnesium chloride;
s6: and (4) spray-drying the humate solution obtained in the S5 to obtain humate powder, carrying out compound reaction on the humate powder and a microbial agent by using a fluidized bed, and controlling the temperature of a compound of the fluidized bed to be 55-75 ℃ according to different microbial agent temperature tolerance conditions to obtain a qualified product.
2. The preparation method of the organic water-soluble bacterial fertilizer with high hard water resistance as claimed in claim 1, wherein the initiator in S1 is 4% of potassium persulfate.
3. The preparation method of the organic water-soluble bacterial fertilizer with high hard water resistance according to claim 1, wherein the secondary centrifugal separation equipment used in S2 is a horizontal centrifuge or a butterfly centrifuge.
4. The preparation method of the organic water soluble bacterial fertilizer with high hard water resistance according to claim 1, wherein the water content of the product in S6 is 5-12%.
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| CN202110455668.5A CN115246751A (en) | 2021-04-26 | 2021-04-26 | Preparation method of high-hard water resistance organic water-soluble bacterial fertilizer |
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Citations (8)
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|---|---|---|---|---|
| FR2383146A1 (en) * | 1977-03-09 | 1978-10-06 | Rodrigues Correia Zulmira | Fertilisers rich in soluble humic acid - prepd. by treating lignite with alkali and a bio-catalyst contg. excrement |
| CN103865002A (en) * | 2014-03-28 | 2014-06-18 | 井冈山大学 | High-water absorption humic acid resin with water conserving, water retention and trace fertilizer sustained-release functions |
| WO2014106423A1 (en) * | 2013-01-05 | 2014-07-10 | 迟英娟 | Method for preparing organic chelate fertilizer |
| CN106748347A (en) * | 2017-03-30 | 2017-05-31 | 山西广宇通科技股份有限公司 | A kind of method that utilization fluid bed prepares humic acid complex micro organism fungicide |
| CN107445748A (en) * | 2016-05-31 | 2017-12-08 | 辽宁东萌肥业科技有限公司 | The quick-acting micro- fertile preparation methods of state raw coal base humic acid chelating |
| CN109337091A (en) * | 2018-10-23 | 2019-02-15 | 宁夏天鑫源生物科技有限公司 | A kind of hard water resistance humic acid potassium and its preparation method and application |
| CN111548221A (en) * | 2020-06-03 | 2020-08-18 | 郑州大学 | Fulvic acid water-soluble fertilizer crystal inhibitor and preparation method thereof |
| CN112409609A (en) * | 2020-11-24 | 2021-02-26 | 张坤 | Neutral and subacid sulfonated potassium fulvate and preparation method thereof |
-
2021
- 2021-04-26 CN CN202110455668.5A patent/CN115246751A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2383146A1 (en) * | 1977-03-09 | 1978-10-06 | Rodrigues Correia Zulmira | Fertilisers rich in soluble humic acid - prepd. by treating lignite with alkali and a bio-catalyst contg. excrement |
| WO2014106423A1 (en) * | 2013-01-05 | 2014-07-10 | 迟英娟 | Method for preparing organic chelate fertilizer |
| CN103865002A (en) * | 2014-03-28 | 2014-06-18 | 井冈山大学 | High-water absorption humic acid resin with water conserving, water retention and trace fertilizer sustained-release functions |
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| CN106748347A (en) * | 2017-03-30 | 2017-05-31 | 山西广宇通科技股份有限公司 | A kind of method that utilization fluid bed prepares humic acid complex micro organism fungicide |
| CN109337091A (en) * | 2018-10-23 | 2019-02-15 | 宁夏天鑫源生物科技有限公司 | A kind of hard water resistance humic acid potassium and its preparation method and application |
| CN111548221A (en) * | 2020-06-03 | 2020-08-18 | 郑州大学 | Fulvic acid water-soluble fertilizer crystal inhibitor and preparation method thereof |
| CN112409609A (en) * | 2020-11-24 | 2021-02-26 | 张坤 | Neutral and subacid sulfonated potassium fulvate and preparation method thereof |
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| 张艳玲;高建仁;邢士玉;邵光伟;胡兆平;: "褐煤腐植酸氧化改性后的抗硬水性能研究", 山东化工 * |
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