CN105801296A - Production method of nano humic acid cheated manganese fertilizer - Google Patents
Production method of nano humic acid cheated manganese fertilizer Download PDFInfo
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- CN105801296A CN105801296A CN201610135319.4A CN201610135319A CN105801296A CN 105801296 A CN105801296 A CN 105801296A CN 201610135319 A CN201610135319 A CN 201610135319A CN 105801296 A CN105801296 A CN 105801296A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
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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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Abstract
The invention relates to a production method of nano humic acid cheated manganese fertilizer, belonging to the technical field of fertilizer production. In the method, the humic acid is subjected to nano modification by adding a surfactant and combining the high-speed stirring and ultrasonic technology; compared with a common humic acid solution, the active groups and active sites of nano humic acid are exposed in an aqueous solution more sufficiently, the contact frequency between the humic acid and manganese ions can be effectively increased, and the chelation property is greatly improved; moreover, the nano humic acid cheated manganese can be directly absorbed by the plant root system, and thus the utilization rate of the fertilizer is increased; the plant growth can be stimulated, and the crop yield is increased. The method has the advantages of simple technology, flexible operation, low production cost and the like, and thus has relatively great advantages in production technology and economy.
Description
Technical field
The present invention relates to the production method of a kind of nanometer of humic acid chelating manganese fertilizer, belong to technical field of fertilizer manufacture, what be specifically related to is the technical method manufacturing nanometer humic acid chelating manganese fertilizer with humic acids, manganese sulfate or manganese chloride for raw material.
Background technology
Manganese is one of necessary trace element of plant, it participates in the conversion of photosynthesis and nitrogen, participate in activity and the oxidation-reduction process of many enzymes, the operating of chlorophyllous synthesis and carbohydrate can be promoted, therefore, the crop that manganese fertilizer has sound response is a lot, almost includes various crops, fruit tree and vegetable etc..When serious manganese deficiency in soil, there is withered and yellow, undergrowth in crops, and yield declines.Investigation according to Chinese Academy of Sciences Nanjing soil and fertilizer institute and Jiangsu Academy of Agricultural Sciences shows, China's manganese deficiency soil reaches more than hundred million mu, uses manganese fertilizer, obvious effect of increasing production on manganese deficiency soil, if executing lkg manganese fertilizer in annual every mu, China's agricultural just need to reach more than 100,000 t containing manganese fertilizer material.
The manganese fertilizer that China commonly uses has inorganic manganese fertilizer and organic manganese fertilizer, and inorganic manganese fertilizer mainly has manganese sulfate, manganese chloride, manganese nitrate, manganese mud etc., and what agricultural production was commonly used is water miscible manganese sulfate, can be used as base manure, seed soaking, dresses seed and topdress.Affect growth owing to crop manganese deficiency occurs mainly in fertility early stage, therefore manganese fertilizer is preferably used in plant growth early stage, but when inorganic manganese fertilizer is used, there is problems in that (1) manganese is oxidized easily thus reducing utilization rate of fertilizer；(2) manganese is easily lost fertilizer efficiency by soil fixing after being manured into soil.Therefore, preferably using organic manganese fertilizer in actual production, organic manganese fertilizer includes: EDTA Chelated Manganese, chelating amino acids manganese, humic acid chelating manganese etc., organic manganese fertilizer is not easily fixed in soil, and mobility and absorbance in plant are better than far away inorganic manganese fertilizer.Both can individually use, it is possible to mix with other solid-state or liquid fertilizer and use, it is possible to as the raw material of Bulk Blending Fertilizer, and promote other fertilizer utilization, but price is higher.
Nanotechnology is in nanoscale, by the control of substance reaction, transmission and transformation being created new material, device and making full use of their characteristic, and explores the new phenomenon of the motion of matter in nanoscale and new rule.Nano fertilizer is the brand-new fertilizer building with nano material technology, modifiying by medicine microcapsule technology and chemical industry micro-emulsion technology, nano material contained by nano fertilizer has skin effect and small-size effect, effectively strengthen the absorption property of fertilizer, improve utilization rate of fertilizer；Also can fully adsorb and be combined in root system of plant surface, promote the plant absorption to nutrient；Moreover it is possible to improve soil physico-chemical property, strengthen soil and store fertile fertilizer-preserving ability.At present, adopt the technology such as modern ultralow temperature, micronizing, hyperfiltration treatment that humic acids carries out a nano modification preparation nanometer humic acids to have been reported, compared with common humic acid solution, active group and the avtive spot of nanometer humic acids are exposed more fully in aqueous, the contact frequency of humic acids and chelating ion can be effectively increased, chelating ability is greatly improved, but, the production method of nanometer humic acid chelating manganese and have not been reported for agricultural production as trace-element fertilizer.
Summary of the invention
It is an object of the invention to, it is provided that the production method of a kind of nanometer of humic acid chelating manganese fertilizer, for achieving the goal, the present invention by the following technical solutions:
(1) preparation of nitro humic acid: humic acid powder is broken to by 80 mesh sieves, the humic acids weighing certain mass is put in reactor A, add 40wt% salpeter solution, humic acids and salpeter solution mass ratio are 1:(0.3～0.5), carrying out aoxidizing and nitration reaction, the response time is 15～30min, after reaction terminates, filter, with water by insoluble matter washing to neutral；
(2) nitro humic acid is dissolved in aqueous slkali: insoluble matter is transferred to reactor B, and the mass ratio adding 4wt%NaOH solution, humic acids and sodium hydroxide solution is 1:10～15, and mixing speed is 300～500r/min, stirs 20～40min；
(3) preparation of Chelated Manganese and spray-drying process: regulating (2) gained pH value of solution with 1mol/L sulfuric acid solution is 6～8, add surfactant, high-speed stirred under ul-trasonic irradiation, mixing speed is 3000～5000r/min, ultrasonic frequency is 60kHz, 10wt% manganese sulfate or manganese chloride solution it is uniformly added into pump, the mass ratio of humic acids and manganese sulfate or manganese chloride is 1.5～4.5:1,30min adds complete, in reactor, solution temperature ranges is 80～120 DEG C, high-speed stirred 1～4h, obtains containing a nanometer suspension for humic acid chelating manganese；Carrying out spray drying under ul-trasonic irradiation, ultrasonic frequency is 60kHz, and inlet temperature is 180～200 DEG C, and leaving air temp is 80～100 DEG C, obtains a nanometer humic acid chelating manganese powder end.
Described surfactant is: polyoxyethylene aliphatic alcohol ether, and poly-(ethylene) 5 nonyl ethers, ethylene glycol nonylplenyl ether, alkyl phenol ethylene oxide, one or more in span Tween 80 carry out composite in proportion.
In the present invention make consumption be product quality the 0.15～0.7% of surfactant.
In the present invention, the Fe content of nanometer humic acid chelating manganese is between 2～15wt%.
Present invention process technology has the advantage that
1, the present invention finds a kind of new method producing nanometer humic acid chelating manganese fertilizer, utilizes this explained hereafter nanometer humic acid chelating manganese and has no report as trace-element fertilizer for agricultural production.
2, nanometer humic acid chelating manganese that the present invention produces, owing to humic acids is carried out nano modification, compared with common humic acid solution, active group and the avtive spot of nanometer humic acids are exposed more fully in aqueous, being effectively increased the contact frequency of humic acids and manganese ion, chelating ability is greatly improved.
3 compared with common humic acid chelating manganese fertilizer, nanometer humic acid chelating manganese that the present invention produces, and size is little, and activity is high, it is possible to directly absorbed by root system of plant, thus improve utilization rate of fertilizer；Also promote the synthesis of plant inner chlorophyll and the operating of carbohydrate, stimulate plant growing, improve crop yield.
4, present invention process has the advantage that production technology is simple, easy to operate, production cost is low.Therefore the present invention in production technology and economically all has greater advantage.
Equilibrium relation between the demand of manganese, nutrient reasonably should be used by the use of nanometer humic acids manganese according to soil characteristic, crop.Base fertilizer should be made use at topsoil, also can with npk fertilizer compounding application.
Edaphic condition and manganese fertilizer are used: the general leading indicator that Active manganese content supplies manganese ability as diagnosis soil, in soil, Active manganese content is extremely low level less than 50mg/kg, content 50mg/kg-100mg/kg is low, 100mg/kg-200mg/kg is medium, 200mg/kg-300mg/kg horn of plenty, is very abundant more than 300mg/kg.Using manganese fertilizer on the soil of manganese deficiency, general crop has good effect of increasing production.
When base manure is used, nanometer humic acid chelating manganese fertilizer being 15% for Fe content, general 666.7 square area year amount of application be 0.6-2.5kg.
Detailed description of the invention
By following instance, the process of the present invention is described.But, example is not limitation of the present invention.
Example 1.
(1) preparation of nitro humic acid: be broken to humic acid powder by 80 mesh sieves, weighs 5kg humic acids and puts in reactor A, adds 1.65kg40wt% salpeter solution, carrying out aoxidizing and nitration reaction, the response time is 15min, after reaction terminates, filter, with water by insoluble matter washing to neutral；
(2) nitro humic acid is dissolved in aqueous slkali: insoluble matter is transferred to reactor B, adds 55kg4wt%NaOH solution, and mixing speed is 320r/min, stirs 25min；
(3) preparation of Chelated Manganese and spray-drying process: regulating (2) gained pH value of solution with 1mol/L sulfuric acid solution is 6.5, add 8.55g polyoxyethylene aliphatic alcohol ether, high-speed stirred under ul-trasonic irradiation, mixing speed is 3500r/min, and ultrasonic frequency is 60kHz, is uniformly added into 11.63kg10wt% manganese sulfate solution with pump, 30min adds complete, in reactor, solution temperature ranges is 85 DEG C, high-speed stirred 1.5h, obtains containing a nanometer suspension for humic acids manganese；Carrying out spray drying under ul-trasonic irradiation, ultrasonic frequency is 60kHz, and inlet temperature is 180 DEG C, and leaving air temp is 85 DEG C, obtains 3.42kg nanometer of humic acids manganese powder end, and Fe content is 5%.
Example 2.
(1) preparation of nitro humic acid: be broken to humic acid powder by 80 mesh sieves, weighs 10kg humic acids and puts in reactor A, adds 4kg40wt% salpeter solution, carrying out aoxidizing and nitration reaction, the response time is 25min, after reaction terminates, filter, with water by insoluble matter washing to neutral；
(2) nitro humic acid is dissolved in aqueous slkali: insoluble matter is transferred to reactor B, adds 120kg4wt%NaOH solution, and mixing speed is 400r/min, and mixing time is 30min；
(3) preparation of Chelated Manganese and spray-drying process: regulating (2) gained pH value of solution with 1mol/L sulfuric acid solution is 7.0, add 33.3g surfactant, surfactant is poly-(ethylene) 5 nonyl ethers, the mixture of ethylene glycol nonylplenyl ether and alkyl phenol ethylene oxide, three's mass ratio is 1:1:1, high-speed stirred under ul-trasonic irradiation, mixing speed is 3800r/min, ultrasonic frequency is 60kHz, it is uniformly added into 32kg10wt% manganese chloride solution with pump, 30min adds complete, in reactor, solution temperature is 90 DEG C, high-speed stirred 2.5h, obtain containing a nanometer suspension for humic acids manganese；Carrying out spray drying under ul-trasonic irradiation, ultrasonic frequency is 60kHz, and inlet temperature is 190 DEG C, and leaving air temp is 90 DEG C, obtains 7.40kg nanometer of humic acids manganese powder end, and Fe content is 8wt%.
Example 3.
(1) preparation of nitro humic acid: be broken to humic acid powder by 80 mesh sieves, weighs 20kg humic acids and puts in reactor A, adds 7.6kg40wt% salpeter solution, carrying out aoxidizing and nitration reaction, the response time is 30min, after reaction terminates, filter, with water by insoluble matter washing to neutral；
(2) nitro humic acid is dissolved in aqueous slkali: insoluble matter is transferred to reactor B, adds 260kg4wt%NaOH solution, and mixing speed is 450r/min, and mixing time is 35min；
(3) preparation of Chelated Manganese and spray-drying process: regulating (2) gained pH value of solution with 1mol/L sulfuric acid solution is 7.5, add surfactant 77.8g, surfactant is the mixture of poly-(ethylene) 5 nonyl ethers with span tween, both mass ratioes are 1:2, high-speed stirred under ul-trasonic irradiation, mixing speed is 4000r/min, ultrasonic frequency is 60kHz, it is uniformly added into 72kg10wt% manganese sulfate solution with pump, 30min adds complete, in reactor, solution temperature is 95 DEG C, high-speed stirred 3h, obtains containing a nanometer suspension for humic acids manganese；Carrying out spray drying under ul-trasonic irradiation, ultrasonic frequency is 60kHz, and inlet temperature is 190 DEG C, and leaving air temp is 85 DEG C, obtains 15.56kg nanometer of humic acids manganese powder end, and Fe content is 10wt%.
Example 4.
(1) preparation of nitro humic acid: be broken to humic acid powder by 80 mesh sieves, weighs 50kg humic acids and puts in reactor A, adds 22.5kg40wt% salpeter solution, carrying out aoxidizing and nitration reaction, the response time is 25min, after reaction terminates, filter, with water by insoluble matter washing to neutral；
(2) nitro humic acid is dissolved in aqueous slkali: insoluble matter is transferred to reactor B, adds 700kg4wt%NaOH solution, and mixing speed is 500r/min, and mixing time is 40min；
(3) preparation of Chelated Manganese and spray-drying process: regulating (2) gained pH value of solution with 1mol/L sulfuric acid solution is 8, add surfactant 264.72g, surfactant is poly-(ethylene) 5 nonyl ethers, the mixture of polyoxyethylene aliphatic alcohol ether and ethylene glycol nonylplenyl ether, three's mass ratio is 1:2:3, high-speed stirred under ul-trasonic irradiation, mixing speed is 4500r/min, ultrasonic frequency is 60kHz, it is uniformly added into 307.7kg10wt% manganese chloride solution with pump, 30min adds complete, in reactor, solution temperature is 110 DEG C, high-speed stirred 3.5h, obtain containing a nanometer suspension for humic acids manganese；Carrying out spray drying under ul-trasonic irradiation, ultrasonic frequency is 60kHz, and inlet temperature is 200 DEG C, and leaving air temp is 90 DEG C, obtains 44.12kg nanometer of humic acids manganese powder end, and Fe content is 15wt%.
Claims (2)
1. the production method of one kind of nanometer of humic acid chelating manganese fertilizer, it is characterised in that its preparation process is:
(1) preparation of nitro humic acid: humic acid powder is broken to by 80 mesh sieves, the humic acids weighing certain mass is put in reactor A, add 40wt% salpeter solution, humic acids and salpeter solution mass ratio are 1:(0.3～0.5), carrying out aoxidizing and nitration reaction, the response time is 15～30min, after reaction terminates, filter, with water by insoluble matter washing to neutral；
(2) nitro humic acid is dissolved in aqueous slkali: insoluble matter is transferred to reactor B, and the mass ratio adding 4wt%NaOH solution, humic acids and sodium hydroxide solution is 1:10～15, and mixing speed is 300～500r/min, stirs 20～40min；
(3) preparation of Chelated Manganese and spray-drying process: regulating (2) gained pH value of solution with 1mol/L sulfuric acid solution is 6～8, add surfactant, high-speed stirred under ul-trasonic irradiation, mixing speed is 3000～5000r/min, ultrasonic frequency is 60KHz, 10wt% manganese sulfate or manganese chloride solution it is uniformly added into pump, the mass ratio of humic acids and manganese sulfate or manganese chloride is 4.5～1.5:1,30min adds complete, in reactor, solution temperature ranges is 80～120 DEG C, high-speed stirred 1～4h, obtains containing a nanometer suspension for humic acids manganese；Carrying out spray drying under ul-trasonic irradiation, ultrasonic frequency is 60KHz, and inlet temperature is 180～200 DEG C, and leaving air temp is 80～100 DEG C, obtains a nanometer humic acids manganese powder end, and Fe content is adjustable between 2～15wt%；
Described surfactant is: polyoxyethylene aliphatic alcohol ether, and poly-(ethylene) 5 nonyl ethers, ethylene glycol nonylplenyl ether, alkyl phenol ethylene oxide, one or more in span Tween 80 carry out composite in proportion.
2. a production method for as claimed in claim 1 nanometer of humic acid chelating manganese fertilizer, make consumption be product quality the 0.15～0.7% of described surfactant.
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Citations (6)
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| CN1275554A (en) * | 1999-05-31 | 2000-12-06 | 第五思军 | High potassium organic compound fertilizer and making method thereof |
| CN101225005A (en) * | 2008-02-01 | 2008-07-23 | 山东省林业科学研究院 | Humic acid slowly available fertilizer and preparation method thereof |
| CN101768031A (en) * | 2009-12-30 | 2010-07-07 | 马增禄 | Preparation method of humic acid organic fertilizer |
| CN104945201A (en) * | 2015-07-03 | 2015-09-30 | 赵海银 | Technical method for preparing oxygen-source efficient humic acid and ecological environment-friendly multifunctional compound fertilizer and product |
| CN105152816A (en) * | 2015-10-21 | 2015-12-16 | 天津芦阳化肥股份有限公司 | Humic acid chelating slow-release fertilizer special for soybeans and preparation method thereof |
| CN105272739A (en) * | 2015-10-13 | 2016-01-27 | 辽宁嘉吉作物营养有限公司 | Humic acid chelated medium-trace element fertilizer and preparation method thereof |
-
2016
- 2016-03-10 CN CN201610135319.4A patent/CN105801296A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1275554A (en) * | 1999-05-31 | 2000-12-06 | 第五思军 | High potassium organic compound fertilizer and making method thereof |
| CN101225005A (en) * | 2008-02-01 | 2008-07-23 | 山东省林业科学研究院 | Humic acid slowly available fertilizer and preparation method thereof |
| CN101768031A (en) * | 2009-12-30 | 2010-07-07 | 马增禄 | Preparation method of humic acid organic fertilizer |
| CN104945201A (en) * | 2015-07-03 | 2015-09-30 | 赵海银 | Technical method for preparing oxygen-source efficient humic acid and ecological environment-friendly multifunctional compound fertilizer and product |
| CN105272739A (en) * | 2015-10-13 | 2016-01-27 | 辽宁嘉吉作物营养有限公司 | Humic acid chelated medium-trace element fertilizer and preparation method thereof |
| CN105152816A (en) * | 2015-10-21 | 2015-12-16 | 天津芦阳化肥股份有限公司 | Humic acid chelating slow-release fertilizer special for soybeans and preparation method thereof |
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Application publication date: 20160727 |